# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 #============================================================ _audit_creation_date 'August 20, 2006' _audit_creation_method 'from NRCVAX CIF routine and SHELXL97 with Word-Perfect Macro PREP8' _audit_update_record ; May 08, 2007 Assembled, pass-1 May 09, 2007 Text added by JFG ; #============================================================ # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr. John F. Gallagher' _publ_contact_author_address ; School of Chemical Sciences, Dublin City University, Dublin 9, Ireland ; _publ_contact_author_phone '353 1 7005114' _publ_contact_author_fax '353 1 7005503' _publ_contact_author_email john.gallagher@dcu.ie _publ_requested_category CO _publ_requested_coeditor_name 'New Journal of Chemistry' _publ_contact_letter ; May 09, 2007 Please consider this CIF submission as a deposition CIF file for archive on the Cambridge Structural Database. The CIF contains a crystal structure with data collected at room temperature and at low temperature: it is written for publication in the RSC journal New Journal of Chemistry submitted recently in 2007. The CIFs has passed the Chester CHECKCIF routines and gives a satisfactory PRINTCIF file and especially for the low-temperature dataset. The room temperature dataset was on a weakly diffracting crystal with an average intensity reflection of 2 x sigma(I) between 2 and 25 degrees! The crystal barely diffracted on our in-house Bruker P4 diffractometer. The refinement is with restraints using DFIX, ISOR, SIMU and DELU. The low temperature dataser is of higher quality (Southampton X-ray service) and is the subject of major discussion in the NJC paper. The Alert A/B/C's are minimized in the higher quality low-temperature study. The following information should be placed in the EXTRA INFORMATION section for the structural file. Both datasets were obtained on weakly difracting crystals at room temperature (in house P4 diffractometer) and low-temperature (Southampton X-ray service). Regards, John Gallagher ; _publ_section_title ; A Substituted BF2-Chelated Tetraarylazadipyrromethene as an Intrinsic Dual Chemosensor in the 650-850 nm Spectral Range ; loop_ _publ_author_name _publ_author_address J.F.Gallagher ; School of Chemical Sciences, Dublin City University, Dublin 9, Ireland ; J.Killoran ; Conway Institute of Biomolecular and Biomedical Research, Department of Chemistry, University College Dublin, Dublin 4, Ireland ; D.F.O'Shea ; Conway Institute of Biomolecular and Biomedical Research, Department of Chemistry, University College Dublin, Dublin 4, Ireland ; #=========================================================== # 4. TEXT _publ_section_abstract ; The title compound is a BF~2~ chelate macrocycle. ; _publ_section_comment ; Molecular recognition continues to be of major interest. ; _publ_section_exptl_prep ; The title compound (I) has been synthesised as described previously. ; _publ_section_exptl_refinement ; Molecule (I) crystallised in the triclinic system; space group P\=1 assumed and confirmed by the analysis. ; _publ_section_references ; Allen, F.H., (2002). Acta Cryst. B58, 380--388. Burnett, M.N. & Johnson, C.K. (1996). ORTEPIII. Report ORNL-6895, U.S.A. Desiraju & Steiner, 1999, The weak interaction in Chemistry and Biology. Ferguson, G. (1998). PREP8. University of Guelph, Canada. Sheldrick, G.M. (1997). SHELXS97 & SHELXL97. University of G\"ottingen, Germany. Spek, A.L. (2002). PLATON. University of Utrecht, Utrecht, The Netherlands. ; _publ_section_figure_captions ; Fig. 1. A view of the major orientation macrocycle in (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for compound (I) Table 2. Hydrogen bond parameters (major site only) (\%A, \%) for compound (I) ; _publ_section_acknowledgements ; J.F.G. thanks Dublin City University for the purchase of a diffractometer and computer system. The EPSRC (Southampton) is thanked for the low-temperature dataset of (I). ; data_(Ia) _database_code_depnum_ccdc_archive 'CCDC 646558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 532 _chemical_formula_moiety 'C36 H32 B F2 N5' _chemical_formula_sum 'C36 H32 B F2 N5' _chemical_formula_weight 583.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.372(10) _cell_length_b 14.250(13) _cell_length_c 21.168(15) _cell_angle_alpha 106.19(8) _cell_angle_beta 91.03(11) _cell_angle_gamma 92.06(9) _cell_volume 3001(5) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 55 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 10.1 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.963 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker-AXS P4' _diffrn_measurement_method \w _diffrn_standards_number 4 _diffrn_standards_interval_count 296 _diffrn_standards_decay_% 'variation 1' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -1 1 2 -2 3 1 3 -5 -1 1 -3 _diffrn_reflns_number 6853 _diffrn_reflns_av_R_equivalents 0.250 _diffrn_reflns_av_sigmaI/netI 0.465 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 21.1 _reflns_number_total 6401 _reflns_number_gt 1492 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'XSCANS (Bruker-AXS, 1994)' _computing_cell_refinement 'XSCANS (Bruker-AXS, 1994)' _computing_data_reduction 'XSCANS (Bruker-AXS, 1994)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1998)' _computing_publication_material 'SHELXL97 and PREP8 (Ferguson, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1921P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6401 _refine_ls_number_parameters 801 _refine_ls_number_restraints 444 _refine_ls_R_factor_all 0.4138 _refine_ls_R_factor_gt 0.1541 _refine_ls_wR_factor_ref 0.4920 _refine_ls_wR_factor_gt 0.3428 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1A F 0.2504(11) 0.1754(8) 0.2322(6) 0.054(4) Uani 1 1 d . . . F2A F 0.4240(12) 0.2556(10) 0.2039(6) 0.078(5) Uani 1 1 d . . . N1A N 0.3816(16) -0.0105(13) 0.0729(9) 0.047(5) Uani 1 1 d . . . C1A C 0.447(2) -0.0005(17) 0.1305(12) 0.050(6) Uani 1 1 d U . . N2A N 0.4359(17) 0.0806(12) 0.1844(9) 0.051(5) Uani 1 1 d U . . B1A B 0.350(3) 0.170(2) 0.1848(15) 0.052(6) Uani 1 1 d U . . N3A N 0.2854(18) 0.1476(13) 0.1174(9) 0.053(5) Uani 1 1 d U . . C2A C 0.304(2) 0.0610(16) 0.0655(12) 0.046(5) Uani 1 1 d U . . C3A C 0.535(2) -0.0687(17) 0.1395(11) 0.044(5) Uani 1 1 d U . . C4A C 0.586(2) -0.0179(16) 0.2023(11) 0.055(6) Uani 1 1 d U . . H4A H 0.6506 -0.0426 0.2232 0.066 Uiso 1 1 calc R . . C5A C 0.533(2) 0.0698(16) 0.2305(12) 0.049(6) Uani 1 1 d U . . C6A C 0.197(2) 0.2005(18) 0.0958(12) 0.054(6) Uani 1 1 d U . . C7A C 0.162(2) 0.1457(16) 0.0312(12) 0.057(6) Uani 1 1 d U . . H7A H 0.1028 0.1653 0.0044 0.068 Uiso 1 1 calc R . . C8A C 0.229(2) 0.0555(16) 0.0114(13) 0.049(6) Uani 1 1 d U . . C11A C 0.561(3) 0.1367(19) 0.2968(12) 0.063(6) Uani 1 1 d U . . C12A C 0.684(2) 0.1235(18) 0.3222(12) 0.069(6) Uani 1 1 d U . . H12A H 0.7410 0.0789 0.2988 0.082 Uiso 1 1 calc R . . C13A C 0.711(2) 0.1851(17) 0.3871(12) 0.056(6) Uani 1 1 d U . . H13A H 0.7896 0.1785 0.4072 0.067 Uiso 1 1 calc R . . C14A C 0.629(2) 0.2542(17) 0.4221(13) 0.065(6) Uani 1 1 d U . . H14A H 0.6565 0.2964 0.4624 0.078 Uiso 1 1 calc R . . C15A C 0.504(3) 0.2609(18) 0.3967(12) 0.065(6) Uani 1 1 d U . . H15A H 0.4431 0.3004 0.4216 0.078 Uiso 1 1 calc R . . C16A C 0.477(2) 0.2049(17) 0.3321(12) 0.060(6) Uani 1 1 d U . . H16A H 0.3993 0.2134 0.3119 0.072 Uiso 1 1 calc R . . C21A C 0.573(2) -0.1576(17) 0.0973(11) 0.049(5) Uani 1 1 d U . . C22A C 0.492(2) -0.2081(17) 0.0463(11) 0.056(6) Uani 1 1 d U . . H22A H 0.4136 -0.1809 0.0405 0.067 Uiso 1 1 calc R . . C23A C 0.519(2) -0.2992(17) 0.0021(12) 0.060(6) Uani 1 1 d U . . H23A H 0.4640 -0.3298 -0.0333 0.072 Uiso 1 1 calc R . . C24A C 0.638(3) -0.3427(19) 0.0143(14) 0.067(6) Uani 1 1 d U . . C25A C 0.710(2) -0.2920(18) 0.0703(13) 0.069(6) Uani 1 1 d U . . H25A H 0.7792 -0.3230 0.0826 0.083 Uiso 1 1 calc R . . C26A C 0.686(2) -0.2019(17) 0.1078(12) 0.056(6) Uani 1 1 d U . . H26A H 0.7456 -0.1691 0.1407 0.068 Uiso 1 1 calc R . . C27A C 0.780(3) -0.476(2) -0.0174(14) 0.111(11) Uani 1 1 d U . . H27A H 0.8488 -0.4282 -0.0139 0.167 Uiso 1 1 calc R . . H27B H 0.7926 -0.5314 -0.0545 0.167 Uiso 1 1 calc R . . H27C H 0.7784 -0.4971 0.0220 0.167 Uiso 1 1 calc R . . N24A N 0.660(2) -0.4345(17) -0.0258(12) 0.095(8) Uani 1 1 d U . . C28A C 0.584(3) -0.4816(19) -0.0837(14) 0.107(10) Uani 1 1 d U . . H28A H 0.4976 -0.4944 -0.0716 0.161 Uiso 1 1 calc R . . H28B H 0.6213 -0.5422 -0.1060 0.161 Uiso 1 1 calc R . . H28C H 0.5818 -0.4399 -0.1123 0.161 Uiso 1 1 calc R . . C31A C 0.135(3) 0.2914(18) 0.1241(11) 0.059(8) Uani 1 1 d . . . C32A C 0.188(3) 0.353(2) 0.1837(16) 0.091(11) Uani 1 1 d . . . H32A H 0.2601 0.3366 0.2044 0.109 Uiso 1 1 calc R . . C33A C 0.131(4) 0.436(2) 0.2085(14) 0.095(12) Uani 1 1 d . . . H33A H 0.1755 0.4836 0.2419 0.114 Uiso 1 1 calc R . . C34A C 0.009(3) 0.4596(19) 0.1889(15) 0.084(11) Uani 1 1 d . . . H34A H -0.0324 0.5149 0.2124 0.101 Uiso 1 1 calc R . . C35A C -0.044(3) 0.398(3) 0.1352(19) 0.117(13) Uani 1 1 d . . . H35A H -0.1211 0.4143 0.1182 0.140 Uiso 1 1 calc R . . C36A C 0.012(3) 0.311(2) 0.1032(14) 0.075(9) Uani 1 1 d . . . H36A H -0.0323 0.2664 0.0683 0.090 Uiso 1 1 calc R . . C41A C 0.217(2) -0.021(2) -0.0499(12) 0.055(8) Uani 1 1 d . . . C42A C 0.116(3) -0.022(2) -0.0909(13) 0.074(9) Uani 1 1 d . . . H42A H 0.0564 0.0267 -0.0797 0.089 Uiso 1 1 calc R . . C43A C 0.098(2) -0.0979(17) -0.1517(11) 0.056(7) Uani 1 1 d . . . H43A H 0.0263 -0.0987 -0.1788 0.067 Uiso 1 1 calc R . . C44A C 0.190(2) -0.1725(17) -0.1711(13) 0.046(6) Uani 1 1 d U . . C45A C 0.291(2) -0.1616(19) -0.1250(13) 0.059(8) Uani 1 1 d . . . H45A H 0.3537 -0.2084 -0.1353 0.071 Uiso 1 1 calc R . . C46A C 0.310(2) -0.0938(18) -0.0689(14) 0.063(8) Uani 1 1 d . . . H46A H 0.3825 -0.0934 -0.0421 0.075 Uiso 1 1 calc R . . C47A C 0.263(2) -0.3199(17) -0.2482(12) 0.071(8) Uani 1 1 d U . . H47A H 0.3448 -0.2916 -0.2549 0.106 Uiso 1 1 calc R . . H47B H 0.2328 -0.3669 -0.2882 0.106 Uiso 1 1 calc R . . H47C H 0.2710 -0.3516 -0.2139 0.106 Uiso 1 1 calc R . . N44A N 0.1712(18) -0.2441(15) -0.2295(10) 0.065(6) Uani 1 1 d U . . C48A C 0.056(2) -0.245(2) -0.2698(13) 0.091(9) Uani 1 1 d U . . H48A H -0.0194 -0.2443 -0.2439 0.137 Uiso 1 1 calc R . . H48B H 0.0519 -0.3024 -0.3065 0.137 Uiso 1 1 calc R . . H48C H 0.0583 -0.1877 -0.2856 0.137 Uiso 1 1 calc R . . F1B F 0.0990(12) 0.2770(8) 0.6910(6) 0.062(4) Uani 1 1 d . . . F2B F 0.2339(12) 0.1978(10) 0.7422(6) 0.068(4) Uani 1 1 d . . . N1B N 0.1318(18) 0.0068(14) 0.5783(10) 0.058(6) Uani 1 1 d . . . C1B C 0.052(2) 0.0172(16) 0.6236(11) 0.044(5) Uani 1 1 d U . . N2B N 0.0580(17) 0.1041(12) 0.6803(8) 0.044(4) Uani 1 1 d U . . B1B B 0.156(3) 0.194(2) 0.6840(14) 0.049(6) Uani 1 1 d U . . N3B N 0.2428(18) 0.1613(14) 0.6250(9) 0.059(5) Uani 1 1 d U . . C2B C 0.227(2) 0.0716(18) 0.5728(12) 0.063(6) Uani 1 1 d U . . C3B C -0.047(2) -0.0456(17) 0.6340(11) 0.047(6) Uani 1 1 d U . . C4B C -0.093(2) -0.0079(16) 0.6948(12) 0.059(6) Uani 1 1 d U . . H4B H -0.1546 -0.0376 0.7154 0.070 Uiso 1 1 calc R . . C5B C -0.032(2) 0.0839(16) 0.7211(12) 0.055(6) Uani 1 1 d U . . C6B C 0.342(2) 0.2146(17) 0.6019(13) 0.061(6) Uani 1 1 d U . . C7B C 0.382(2) 0.1625(15) 0.5447(11) 0.047(5) Uani 1 1 d U . . H7B H 0.4470 0.1840 0.5215 0.057 Uiso 1 1 calc R . . C8B C 0.314(2) 0.0672(17) 0.5216(12) 0.054(6) Uani 1 1 d U . . C11B C -0.053(2) 0.1512(16) 0.7932(13) 0.058(6) Uani 1 1 d U . . C12B C -0.113(2) 0.1032(18) 0.8333(12) 0.062(6) Uani 1 1 d U . . H12B H -0.1363 0.0369 0.8194 0.074 Uiso 1 1 calc R . . C13B C -0.136(2) 0.1638(18) 0.8992(12) 0.055(6) Uani 1 1 d U . . H13B H -0.1712 0.1342 0.9292 0.066 Uiso 1 1 calc R . . C14B C -0.110(2) 0.2597(18) 0.9186(13) 0.060(6) Uani 1 1 d U . . H14B H -0.1279 0.2969 0.9609 0.072 Uiso 1 1 calc R . . C15B C -0.056(2) 0.3006(18) 0.8751(13) 0.064(6) Uani 1 1 d U . . H15B H -0.0360 0.3674 0.8896 0.077 Uiso 1 1 calc R . . C16B C -0.026(2) 0.2524(16) 0.8096(13) 0.067(6) Uani 1 1 d U . . H16B H 0.0081 0.2843 0.7804 0.080 Uiso 1 1 calc R . . C21B C -0.075(2) -0.1458(19) 0.5870(13) 0.063(6) Uani 1 1 d U . . C22B C -0.045(2) -0.1674(18) 0.5221(12) 0.062(6) Uani 1 1 d U . . H22B H -0.0127 -0.1172 0.5059 0.074 Uiso 1 1 calc R . . C23B C -0.061(2) -0.2615(17) 0.4789(12) 0.061(6) Uani 1 1 d U . . H23B H -0.0361 -0.2730 0.4354 0.074 Uiso 1 1 calc R . . C24B C -0.114(2) -0.3399(19) 0.5010(13) 0.064(6) Uani 1 1 d U . . C25B C -0.149(2) -0.3146(19) 0.5674(13) 0.065(6) Uani 1 1 d U . . H25B H -0.1819 -0.3631 0.5850 0.079 Uiso 1 1 calc R . . C26B C -0.135(2) -0.2215(19) 0.6066(13) 0.067(6) Uani 1 1 d U . . H26B H -0.1670 -0.2076 0.6488 0.081 Uiso 1 1 calc R . . C27B C -0.191(3) -0.5094(19) 0.4884(15) 0.117(11) Uani 1 1 d U . . H27D H -0.2011 -0.5706 0.4548 0.175 Uiso 1 1 calc R . . H27E H -0.2738 -0.4892 0.5054 0.175 Uiso 1 1 calc R . . H27F H -0.1357 -0.5170 0.5234 0.175 Uiso 1 1 calc R . . N24B N -0.131(3) -0.4320(18) 0.4592(13) 0.103(8) Uani 1 1 d U . . C28B C -0.086(3) -0.459(2) 0.3895(12) 0.095(9) Uani 1 1 d U . . H28D H 0.0064 -0.4497 0.3897 0.143 Uiso 1 1 calc R . . H28E H -0.1251 -0.4179 0.3662 0.143 Uiso 1 1 calc R . . H28F H -0.1100 -0.5261 0.3683 0.143 Uiso 1 1 calc R . . C31B C 0.390(2) 0.3148(17) 0.6382(14) 0.054(7) Uani 1 1 d . . . C32B C 0.387(3) 0.365(2) 0.7095(15) 0.104(11) Uani 1 1 d . . . H32B H 0.3570 0.3313 0.7386 0.124 Uiso 1 1 calc R . . C33B C 0.430(3) 0.4605(19) 0.7325(15) 0.083(10) Uani 1 1 d . . . H33B H 0.4234 0.4939 0.7768 0.100 Uiso 1 1 calc R . . C34B C 0.483(3) 0.507(2) 0.6896(17) 0.091(11) Uani 1 1 d . . . H34B H 0.5186 0.5699 0.7071 0.109 Uiso 1 1 calc R . . C35B C 0.487(3) 0.4659(19) 0.6217(17) 0.090(10) Uani 1 1 d . . . H35B H 0.5204 0.5012 0.5943 0.108 Uiso 1 1 calc R . . C36B C 0.439(2) 0.3691(18) 0.5968(12) 0.065(8) Uani 1 1 d . . . H36B H 0.4401 0.3397 0.5517 0.079 Uiso 1 1 calc R . . C41B C 0.325(2) -0.0078(18) 0.4629(13) 0.058(7) Uani 1 1 d . . . C42B C 0.391(2) 0.0022(18) 0.4094(14) 0.055(7) Uani 1 1 d . . . H42B H 0.4341 0.0624 0.4147 0.066 Uiso 1 1 calc R . . C43B C 0.401(2) -0.062(2) 0.3520(13) 0.065(8) Uani 1 1 d . . . H43B H 0.4473 -0.0462 0.3187 0.078 Uiso 1 1 calc R . . C44B C 0.336(2) -0.1601(18) 0.3421(13) 0.062(7) Uani 1 1 d U . . C45B C 0.274(2) -0.1774(17) 0.3971(12) 0.055(7) Uani 1 1 d . . . H45B H 0.2356 -0.2386 0.3939 0.066 Uiso 1 1 calc R . . C46B C 0.271(3) -0.1046(17) 0.4550(11) 0.071(9) Uani 1 1 d . . . H46B H 0.2314 -0.1184 0.4907 0.086 Uiso 1 1 calc R . . C47B C 0.272(2) -0.3260(17) 0.2792(12) 0.078(8) Uani 1 1 d U . . H47D H 0.1818 -0.3170 0.2869 0.117 Uiso 1 1 calc R . . H47E H 0.3091 -0.3528 0.3119 0.117 Uiso 1 1 calc R . . H47F H 0.2827 -0.3700 0.2363 0.117 Uiso 1 1 calc R . . N44B N 0.337(2) -0.2311(16) 0.2831(11) 0.078(7) Uani 1 1 d U . . C48B C 0.404(2) -0.2194(17) 0.2257(11) 0.062(7) Uani 1 1 d U . . H48D H 0.4905 -0.1946 0.2382 0.094 Uiso 1 1 calc R . . H48E H 0.3590 -0.1742 0.2078 0.094 Uiso 1 1 calc R . . H48F H 0.4053 -0.2815 0.1931 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1A 0.072(9) 0.048(9) 0.048(9) 0.024(7) 0.001(7) 0.003(7) F2A 0.056(9) 0.094(12) 0.062(10) -0.008(9) -0.018(8) -0.022(8) N1A 0.055(13) 0.038(13) 0.054(14) 0.025(11) -0.020(11) -0.002(10) C1A 0.068(11) 0.039(10) 0.041(10) 0.006(9) 0.015(10) -0.019(9) N2A 0.060(10) 0.027(9) 0.058(10) 0.003(8) -0.004(9) -0.023(8) B1A 0.070(12) 0.027(10) 0.058(11) 0.013(10) -0.009(10) -0.015(10) N3A 0.079(11) 0.032(9) 0.050(10) 0.017(8) -0.014(9) -0.016(9) C2A 0.063(11) 0.026(10) 0.052(11) 0.015(9) 0.007(9) -0.012(9) C3A 0.053(12) 0.042(12) 0.037(11) 0.009(10) 0.006(10) 0.003(10) C4A 0.063(12) 0.047(12) 0.053(12) 0.009(11) 0.023(11) -0.005(10) C5A 0.055(12) 0.027(11) 0.064(13) 0.010(10) 0.005(11) -0.012(10) C6A 0.078(13) 0.041(12) 0.046(12) 0.018(10) -0.014(11) -0.004(11) C7A 0.087(13) 0.038(12) 0.049(12) 0.018(11) 0.002(11) -0.004(11) C8A 0.072(13) 0.028(11) 0.056(12) 0.025(11) 0.011(11) -0.008(10) C11A 0.075(14) 0.068(13) 0.043(13) 0.015(11) -0.006(11) -0.025(12) C12A 0.072(13) 0.068(13) 0.062(13) 0.012(11) -0.001(12) -0.007(12) C13A 0.057(13) 0.060(13) 0.051(13) 0.019(11) -0.004(11) -0.001(11) C14A 0.076(14) 0.054(13) 0.064(13) 0.015(11) 0.008(12) -0.008(12) C15A 0.089(14) 0.051(12) 0.054(13) 0.014(11) 0.002(12) -0.004(12) C16A 0.080(14) 0.047(13) 0.051(13) 0.013(11) -0.001(11) -0.024(11) C21A 0.067(13) 0.048(12) 0.043(12) 0.030(10) 0.002(11) 0.005(10) C22A 0.058(13) 0.053(12) 0.050(13) 0.001(11) 0.000(10) 0.011(11) C23A 0.063(13) 0.055(12) 0.061(13) 0.014(11) -0.004(11) 0.000(11) C24A 0.088(13) 0.043(11) 0.070(12) 0.016(10) 0.011(11) 0.018(10) C25A 0.085(13) 0.048(12) 0.083(14) 0.032(11) -0.001(12) 0.034(11) C26A 0.054(12) 0.052(12) 0.061(13) 0.008(11) 0.008(11) 0.031(11) C27A 0.109(19) 0.09(2) 0.10(2) -0.032(16) 0.014(16) 0.037(16) N24A 0.093(16) 0.075(15) 0.099(17) -0.009(13) -0.013(14) 0.029(13) C28A 0.14(2) 0.062(17) 0.099(19) -0.010(15) -0.015(16) -0.013(16) C31A 0.11(2) 0.046(18) 0.008(13) -0.012(13) -0.002(14) 0.013(17) C32A 0.09(2) 0.05(2) 0.12(3) 0.00(2) -0.03(2) 0.033(18) C33A 0.14(3) 0.06(2) 0.08(2) 0.04(2) -0.07(2) -0.08(2) C34A 0.13(3) 0.030(17) 0.07(2) -0.011(16) -0.04(2) -0.019(19) C35A 0.09(3) 0.13(3) 0.13(4) 0.03(3) 0.04(3) 0.02(3) C36A 0.09(2) 0.08(2) 0.07(2) 0.04(2) -0.047(19) -0.009(18) C41A 0.024(15) 0.10(2) 0.037(17) 0.011(16) -0.012(13) -0.005(15) C42A 0.07(2) 0.08(2) 0.06(2) 0.024(19) 0.019(18) -0.021(17) C43A 0.057(17) 0.067(19) 0.030(16) -0.006(14) -0.023(13) -0.002(15) C44A 0.029(13) 0.035(13) 0.076(16) 0.020(11) -0.003(12) -0.009(11) C45A 0.049(18) 0.052(18) 0.07(2) 0.011(16) 0.001(16) -0.016(14) C46A 0.025(15) 0.054(18) 0.11(3) 0.020(18) -0.014(16) 0.005(14) C47A 0.075(16) 0.065(16) 0.063(17) 0.003(13) -0.015(14) -0.008(12) N44A 0.039(12) 0.065(14) 0.074(15) -0.006(11) -0.003(11) 0.002(10) C48A 0.090(17) 0.10(2) 0.079(18) 0.031(16) -0.023(14) -0.027(15) F1B 0.076(9) 0.024(8) 0.081(11) 0.003(7) 0.023(8) -0.001(7) F2B 0.073(9) 0.082(11) 0.051(9) 0.027(8) 0.002(8) -0.029(8) N1B 0.056(14) 0.059(15) 0.062(15) 0.024(12) -0.009(12) -0.027(12) C1B 0.054(11) 0.048(11) 0.029(10) 0.008(9) 0.011(9) 0.004(9) N2B 0.064(10) 0.045(9) 0.022(9) 0.006(8) 0.011(8) -0.007(8) B1B 0.059(11) 0.049(11) 0.036(11) 0.008(10) 0.004(10) -0.016(10) N3B 0.073(10) 0.046(10) 0.052(10) 0.007(8) 0.000(9) -0.016(9) C2B 0.075(11) 0.051(11) 0.059(11) 0.011(9) 0.007(10) -0.006(10) C3B 0.045(12) 0.054(12) 0.035(11) 0.001(11) -0.006(10) -0.001(10) C4B 0.066(13) 0.048(12) 0.053(12) 0.003(11) -0.010(11) -0.010(10) C5B 0.061(12) 0.041(11) 0.052(12) -0.003(10) 0.006(11) -0.015(10) C6B 0.072(13) 0.033(12) 0.064(13) -0.007(11) -0.004(11) -0.010(10) C7B 0.053(12) 0.033(11) 0.053(12) 0.008(10) 0.013(10) -0.011(10) C8B 0.068(13) 0.046(12) 0.046(12) 0.009(11) 0.012(10) -0.001(10) C11B 0.069(13) 0.019(11) 0.084(14) 0.012(11) 0.004(11) 0.001(10) C12B 0.069(13) 0.041(12) 0.074(14) 0.011(11) 0.011(12) 0.009(11) C13B 0.048(11) 0.056(13) 0.060(13) 0.015(11) 0.003(11) 0.008(11) C14B 0.047(12) 0.064(13) 0.070(14) 0.022(12) 0.017(11) -0.007(11) C15B 0.054(12) 0.054(13) 0.074(14) 0.003(11) 0.014(12) -0.021(11) C16B 0.070(12) 0.036(12) 0.088(14) 0.008(11) 0.002(12) -0.007(11) C21B 0.061(12) 0.063(13) 0.063(13) 0.018(12) -0.009(11) -0.023(11) C22B 0.066(12) 0.055(12) 0.056(13) 0.004(11) 0.010(11) -0.029(11) C23B 0.068(12) 0.058(13) 0.049(12) 0.002(11) 0.011(11) -0.024(11) C24B 0.068(12) 0.057(11) 0.062(12) 0.009(10) 0.000(11) -0.023(10) C25B 0.070(12) 0.058(13) 0.066(13) 0.017(11) -0.005(12) -0.030(11) C26B 0.058(12) 0.069(14) 0.071(14) 0.015(12) 0.002(11) -0.017(12) C27B 0.17(2) 0.055(16) 0.12(2) 0.021(16) -0.013(18) -0.030(17) N24B 0.15(2) 0.068(15) 0.088(16) 0.019(13) 0.006(15) -0.002(14) C28B 0.11(2) 0.094(19) 0.058(15) -0.012(14) -0.019(15) -0.021(16) C31B 0.042(15) 0.046(17) 0.09(2) 0.043(17) 0.021(15) 0.004(13) C32B 0.12(3) 0.08(2) 0.09(3) -0.02(2) 0.00(2) -0.02(2) C33B 0.09(2) 0.04(2) 0.09(3) -0.012(18) 0.006(19) -0.033(17) C34B 0.07(2) 0.09(3) 0.10(3) 0.01(2) -0.02(2) -0.031(19) C35B 0.12(3) 0.040(19) 0.11(3) 0.025(19) -0.01(2) -0.025(18) C36B 0.10(2) 0.054(19) 0.045(17) 0.014(15) -0.011(15) -0.026(16) C41B 0.09(2) 0.045(18) 0.053(19) 0.024(16) 0.001(16) 0.013(15) C42B 0.036(15) 0.046(18) 0.08(2) 0.002(17) 0.002(15) 0.004(12) C43B 0.060(18) 0.08(2) 0.06(2) 0.026(18) 0.035(16) 0.000(16) C44B 0.077(17) 0.039(14) 0.061(15) -0.003(12) 0.000(14) 0.014(13) C45B 0.063(18) 0.035(16) 0.061(19) 0.003(15) 0.012(15) -0.013(13) C46B 0.15(3) 0.046(18) 0.014(15) 0.007(14) -0.016(15) -0.046(17) C47B 0.101(18) 0.051(14) 0.073(17) 0.004(13) -0.003(15) -0.002(13) N44B 0.093(15) 0.060(13) 0.071(14) 0.002(11) 0.015(12) -0.028(12) C48B 0.075(16) 0.065(16) 0.053(14) 0.026(13) 0.001(13) 0.010(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1A B1A 1.44(3) . ? F2A B1A 1.37(3) . ? N1A C1A 1.35(3) . ? N1A C2A 1.36(3) . ? C1A N2A 1.39(3) . ? C1A C3A 1.41(3) . ? N2A C5A 1.43(3) . ? N2A B1A 1.58(3) . ? B1A N3A 1.51(3) . ? N3A C6A 1.36(3) . ? N3A C2A 1.43(3) . ? C2A C8A 1.36(3) . ? C3A C4A 1.40(3) . ? C3A C21A 1.41(3) . ? C4A C5A 1.36(3) . ? C4A H4A 0.9300 . ? C5A C11A 1.48(3) . ? C6A C7A 1.41(3) . ? C6A C31A 1.45(3) . ? C7A C8A 1.44(3) . ? C7A H7A 0.9300 . ? C8A C41A 1.44(3) . ? C11A C16A 1.39(3) . ? C11A C12A 1.41(3) . ? C12A C13A 1.43(3) . ? C12A H12A 0.9300 . ? C13A C14A 1.39(3) . ? C13A H13A 0.9300 . ? C14A C15A 1.41(3) . ? C14A H14A 0.9300 . ? C15A C16A 1.39(3) . ? C15A H15A 0.9300 . ? C16A H16A 0.9300 . ? C21A C22A 1.38(3) . ? C21A C26A 1.39(3) . ? C22A C23A 1.42(3) . ? C22A H22A 0.9300 . ? C23A C24A 1.44(3) . ? C23A H23A 0.9300 . ? C24A N24A 1.38(3) . ? C24A C25A 1.39(3) . ? C25A C26A 1.34(3) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C27A N24A 1.43(3) . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? N24A C28A 1.43(3) . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C31A C32A 1.41(3) . ? C31A C36A 1.41(3) . ? C32A C33A 1.32(4) . ? C32A H32A 0.9300 . ? C33A C34A 1.41(4) . ? C33A H33A 0.9300 . ? C34A C35A 1.32(4) . ? C34A H34A 0.9300 . ? C35A C36A 1.39(4) . ? C35A H35A 0.9300 . ? C36A H36A 0.9300 . ? C41A C42A 1.35(3) . ? C41A C46A 1.43(3) . ? C42A C43A 1.43(3) . ? C42A H42A 0.9300 . ? C43A C44A 1.43(3) . ? C43A H43A 0.9300 . ? C44A N44A 1.37(3) . ? C44A C45A 1.39(3) . ? C45A C46A 1.31(3) . ? C45A H45A 0.9300 . ? C46A H46A 0.9300 . ? C47A N44A 1.44(3) . ? C47A H47A 0.9600 . ? C47A H47B 0.9600 . ? C47A H47C 0.9600 . ? N44A C48A 1.46(3) . ? C48A H48A 0.9600 . ? C48A H48B 0.9600 . ? C48A H48C 0.9600 . ? F1B B1B 1.32(3) . ? F2B B1B 1.45(3) . ? N1B C1B 1.26(2) . ? N1B C2B 1.36(3) . ? C1B C3B 1.40(3) . ? C1B N2B 1.46(2) . ? N2B C5B 1.36(2) . ? N2B B1B 1.59(3) . ? B1B N3B 1.52(3) . ? N3B C6B 1.43(3) . ? N3B C2B 1.44(3) . ? C2B C8B 1.41(3) . ? C3B C4B 1.35(3) . ? C3B C21B 1.51(3) . ? C4B C5B 1.40(3) . ? C4B H4B 0.9300 . ? C5B C11B 1.58(3) . ? C6B C7B 1.32(3) . ? C6B C31B 1.48(3) . ? C7B C8B 1.46(3) . ? C7B H7B 0.9300 . ? C8B C41B 1.41(3) . ? C11B C12B 1.37(3) . ? C11B C16B 1.40(3) . ? C12B C13B 1.45(3) . ? C12B H12B 0.9300 . ? C13B C14B 1.33(3) . ? C13B H13B 0.9300 . ? C14B C15B 1.34(3) . ? C14B H14B 0.9300 . ? C15B C16B 1.41(3) . ? C15B H15B 0.9300 . ? C16B H16B 0.9300 . ? C21B C22B 1.37(3) . ? C21B C26B 1.39(3) . ? C22B C23B 1.40(3) . ? C22B H22B 0.9300 . ? C23B C24B 1.43(3) . ? C23B H23B 0.9300 . ? C24B N24B 1.37(3) . ? C24B C25B 1.41(3) . ? C25B C26B 1.35(3) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? C27B N24B 1.53(3) . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? N24B C28B 1.50(3) . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C31B C36B 1.41(3) . ? C31B C32B 1.48(3) . ? C32B C33B 1.37(3) . ? C32B H32B 0.9300 . ? C33B C34B 1.37(4) . ? C33B H33B 0.9300 . ? C34B C35B 1.39(4) . ? C34B H34B 0.9300 . ? C35B C36B 1.40(3) . ? C35B H35B 0.9300 . ? C36B H36B 0.9300 . ? C41B C42B 1.37(3) . ? C41B C46B 1.43(3) . ? C42B C43B 1.31(3) . ? C42B H42B 0.9300 . ? C43B C44B 1.49(3) . ? C43B H43B 0.9300 . ? C44B N44B 1.37(3) . ? C44B C45B 1.42(3) . ? C45B C46B 1.37(3) . ? C45B H45B 0.9300 . ? C46B H46B 0.9300 . ? C47B N44B 1.47(3) . ? C47B H47D 0.9600 . ? C47B H47E 0.9600 . ? C47B H47F 0.9600 . ? N44B C48B 1.45(3) . ? C48B H48D 0.9600 . ? C48B H48E 0.9600 . ? C48B H48F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A N1A C2A 120(2) . . ? N1A C1A N2A 122(2) . . ? N1A C1A C3A 123(2) . . ? N2A C1A C3A 115(2) . . ? C1A N2A C5A 104(2) . . ? C1A N2A B1A 124(2) . . ? C5A N2A B1A 130.5(19) . . ? F2A B1A F1A 108(2) . . ? F2A B1A N3A 115(2) . . ? F1A B1A N3A 108(2) . . ? F2A B1A N2A 110(2) . . ? F1A B1A N2A 109(2) . . ? N3A B1A N2A 107(2) . . ? C6A N3A C2A 108(2) . . ? C6A N3A B1A 128(2) . . ? C2A N3A B1A 124(2) . . ? C8A C2A N1A 125(2) . . ? C8A C2A N3A 112(2) . . ? N1A C2A N3A 122(2) . . ? C4A C3A C21A 129(2) . . ? C4A C3A C1A 99(2) . . ? C21A C3A C1A 132(2) . . ? C5A C4A C3A 116(2) . . ? C5A C4A H4A 122.2 . . ? C3A C4A H4A 122.2 . . ? C4A C5A N2A 106(2) . . ? C4A C5A C11A 128(3) . . ? N2A C5A C11A 126(2) . . ? N3A C6A C7A 106(2) . . ? N3A C6A C31A 135(2) . . ? C7A C6A C31A 119(2) . . ? C6A C7A C8A 112(2) . . ? C6A C7A H7A 124.0 . . ? C8A C7A H7A 124.0 . . ? C2A C8A C41A 129(2) . . ? C2A C8A C7A 102(2) . . ? C41A C8A C7A 129(2) . . ? C16A C11A C12A 122(2) . . ? C16A C11A C5A 125(2) . . ? C12A C11A C5A 112(2) . . ? C11A C12A C13A 114(2) . . ? C11A C12A H12A 123.2 . . ? C13A C12A H12A 123.2 . . ? C14A C13A C12A 124(2) . . ? C14A C13A H13A 117.9 . . ? C12A C13A H13A 117.9 . . ? C13A C14A C15A 120(3) . . ? C13A C14A H14A 119.8 . . ? C15A C14A H14A 119.8 . . ? C16A C15A C14A 116(3) . . ? C16A C15A H15A 121.9 . . ? C14A C15A H15A 121.9 . . ? C15A C16A C11A 123(3) . . ? C15A C16A H16A 118.7 . . ? C11A C16A H16A 118.7 . . ? C22A C21A C26A 118(2) . . ? C22A C21A C3A 119(2) . . ? C26A C21A C3A 123(2) . . ? C21A C22A C23A 124(2) . . ? C21A C22A H22A 118.2 . . ? C23A C22A H22A 118.2 . . ? C22A C23A C24A 117(2) . . ? C22A C23A H23A 121.5 . . ? C24A C23A H23A 121.5 . . ? N24A C24A C25A 127(3) . . ? N24A C24A C23A 117(3) . . ? C25A C24A C23A 116(2) . . ? C26A C25A C24A 125(2) . . ? C26A C25A H25A 117.5 . . ? C24A C25A H25A 117.5 . . ? C25A C26A C21A 120(2) . . ? C25A C26A H26A 120.1 . . ? C21A C26A H26A 120.1 . . ? N24A C27A H27A 109.5 . . ? N24A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? N24A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C24A N24A C28A 124(3) . . ? C24A N24A C27A 118(3) . . ? C28A N24A C27A 117(2) . . ? N24A C28A H28A 109.5 . . ? N24A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? N24A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C32A C31A C36A 118(2) . . ? C32A C31A C6A 118(3) . . ? C36A C31A C6A 123(3) . . ? C33A C32A C31A 117(3) . . ? C33A C32A H32A 121.6 . . ? C31A C32A H32A 121.6 . . ? C32A C33A C34A 126(3) . . ? C32A C33A H33A 117.2 . . ? C34A C33A H33A 117.2 . . ? C35A C34A C33A 116(3) . . ? C35A C34A H34A 121.9 . . ? C33A C34A H34A 121.9 . . ? C34A C35A C36A 122(3) . . ? C34A C35A H35A 119.0 . . ? C36A C35A H35A 119.0 . . ? C35A C36A C31A 120(3) . . ? C35A C36A H36A 120.2 . . ? C31A C36A H36A 120.2 . . ? C42A C41A C46A 119(3) . . ? C42A C41A C8A 119(3) . . ? C46A C41A C8A 122(2) . . ? C41A C42A C43A 121(3) . . ? C41A C42A H42A 119.5 . . ? C43A C42A H42A 119.5 . . ? C42A C43A C44A 121(2) . . ? C42A C43A H43A 119.7 . . ? C44A C43A H43A 119.7 . . ? N44A C44A C45A 128(2) . . ? N44A C44A C43A 119(2) . . ? C45A C44A C43A 113(2) . . ? C46A C45A C44A 128(3) . . ? C46A C45A H45A 115.8 . . ? C44A C45A H45A 115.8 . . ? C45A C46A C41A 118(2) . . ? C45A C46A H46A 120.9 . . ? C41A C46A H46A 120.9 . . ? N44A C47A H47A 109.5 . . ? N44A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? N44A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C44A N44A C47A 119(2) . . ? C44A N44A C48A 119(2) . . ? C47A N44A C48A 121(2) . . ? N44A C48A H48A 109.5 . . ? N44A C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? N44A C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C1B N1B C2B 127(2) . . ? N1B C1B C3B 131(2) . . ? N1B C1B N2B 121(2) . . ? C3B C1B N2B 107.4(19) . . ? C5B N2B C1B 104.0(18) . . ? C5B N2B B1B 134.5(19) . . ? C1B N2B B1B 121.4(18) . . ? F1B B1B F2B 110(2) . . ? F1B B1B N3B 117(2) . . ? F2B B1B N3B 107(2) . . ? F1B B1B N2B 113(2) . . ? F2B B1B N2B 102(2) . . ? N3B B1B N2B 106(2) . . ? C6B N3B C2B 103.2(19) . . ? C6B N3B B1B 130(2) . . ? C2B N3B B1B 126(2) . . ? N1B C2B C8B 130(2) . . ? N1B C2B N3B 117(2) . . ? C8B C2B N3B 113(2) . . ? C4B C3B C1B 109(2) . . ? C4B C3B C21B 128(2) . . ? C1B C3B C21B 122(2) . . ? C3B C4B C5B 107(2) . . ? C3B C4B H4B 126.4 . . ? C5B C4B H4B 126.4 . . ? N2B C5B C4B 112(2) . . ? N2B C5B C11B 123.9(19) . . ? C4B C5B C11B 124(2) . . ? C7B C6B N3B 110(2) . . ? C7B C6B C31B 126(2) . . ? N3B C6B C31B 124(2) . . ? C6B C7B C8B 112(2) . . ? C6B C7B H7B 123.8 . . ? C8B C7B H7B 123.8 . . ? C41B C8B C2B 128(2) . . ? C41B C8B C7B 130(2) . . ? C2B C8B C7B 101(2) . . ? C12B C11B C16B 125(3) . . ? C12B C11B C5B 114(2) . . ? C16B C11B C5B 121(2) . . ? C11B C12B C13B 115(2) . . ? C11B C12B H12B 122.6 . . ? C13B C12B H12B 122.6 . . ? C14B C13B C12B 123(2) . . ? C14B C13B H13B 118.4 . . ? C12B C13B H13B 118.4 . . ? C13B C14B C15B 117(3) . . ? C13B C14B H14B 121.3 . . ? C15B C14B H14B 121.3 . . ? C14B C15B C16B 127(2) . . ? C14B C15B H15B 116.7 . . ? C16B C15B H15B 116.7 . . ? C11B C16B C15B 113(2) . . ? C11B C16B H16B 123.7 . . ? C15B C16B H16B 123.7 . . ? C22B C21B C26B 116(2) . . ? C22B C21B C3B 122(2) . . ? C26B C21B C3B 122(2) . . ? C21B C22B C23B 123(2) . . ? C21B C22B H22B 118.5 . . ? C23B C22B H22B 118.5 . . ? C22B C23B C24B 120(2) . . ? C22B C23B H23B 119.8 . . ? C24B C23B H23B 119.8 . . ? N24B C24B C25B 124(3) . . ? N24B C24B C23B 121(3) . . ? C25B C24B C23B 115(2) . . ? C26B C25B C24B 122(3) . . ? C26B C25B H25B 119.1 . . ? C24B C25B H25B 119.1 . . ? C25B C26B C21B 123(3) . . ? C25B C26B H26B 118.3 . . ? C21B C26B H26B 118.3 . . ? N24B C27B H27D 109.5 . . ? N24B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? N24B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C24B N24B C28B 123(3) . . ? C24B N24B C27B 116(2) . . ? C28B N24B C27B 121(2) . . ? N24B C28B H28D 109.5 . . ? N24B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? N24B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C36B C31B C32B 117(2) . . ? C36B C31B C6B 113(2) . . ? C32B C31B C6B 129(2) . . ? C33B C32B C31B 120(3) . . ? C33B C32B H32B 120.2 . . ? C31B C32B H32B 120.2 . . ? C32B C33B C34B 119(3) . . ? C32B C33B H33B 120.3 . . ? C34B C33B H33B 120.3 . . ? C33B C34B C35B 125(3) . . ? C33B C34B H34B 117.7 . . ? C35B C34B H34B 117.7 . . ? C34B C35B C36B 117(3) . . ? C34B C35B H35B 121.6 . . ? C36B C35B H35B 121.6 . . ? C35B C36B C31B 122(3) . . ? C35B C36B H36B 119.0 . . ? C31B C36B H36B 119.0 . . ? C42B C41B C8B 124(2) . . ? C42B C41B C46B 114(2) . . ? C8B C41B C46B 122(2) . . ? C43B C42B C41B 129(3) . . ? C43B C42B H42B 115.7 . . ? C41B C42B H42B 115.7 . . ? C42B C43B C44B 117(2) . . ? C42B C43B H43B 121.3 . . ? C44B C43B H43B 121.3 . . ? N44B C44B C45B 121(2) . . ? N44B C44B C43B 122(3) . . ? C45B C44B C43B 117(2) . . ? C46B C45B C44B 120(2) . . ? C46B C45B H45B 119.8 . . ? C44B C45B H45B 119.8 . . ? C45B C46B C41B 123(2) . . ? C45B C46B H46B 118.6 . . ? C41B C46B H46B 118.6 . . ? N44B C47B H47D 109.5 . . ? N44B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? N44B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C44B N44B C48B 124(2) . . ? C44B N44B C47B 117(2) . . ? C48B N44B C47B 119(2) . . ? N44B C48B H48D 109.5 . . ? N44B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? N44B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A N1A C1A N2A 1(3) . . . . ? C2A N1A C1A C3A -175(2) . . . . ? N1A C1A N2A C5A -171.5(19) . . . . ? C3A C1A N2A C5A 6(3) . . . . ? N1A C1A N2A B1A -1(3) . . . . ? C3A C1A N2A B1A 176(2) . . . . ? C1A N2A B1A F2A -125(2) . . . . ? C5A N2A B1A F2A 42(3) . . . . ? C1A N2A B1A F1A 117(2) . . . . ? C5A N2A B1A F1A -76(3) . . . . ? C1A N2A B1A N3A 1(3) . . . . ? C5A N2A B1A N3A 168.2(19) . . . . ? F2A B1A N3A C6A -62(4) . . . . ? F1A B1A N3A C6A 59(3) . . . . ? N2A B1A N3A C6A 176(2) . . . . ? F2A B1A N3A C2A 122(2) . . . . ? F1A B1A N3A C2A -117(2) . . . . ? N2A B1A N3A C2A 0(3) . . . . ? C1A N1A C2A C8A -176(2) . . . . ? C1A N1A C2A N3A -1(3) . . . . ? C6A N3A C2A C8A -1(3) . . . . ? B1A N3A C2A C8A 176(2) . . . . ? C6A N3A C2A N1A -176.2(19) . . . . ? B1A N3A C2A N1A 1(3) . . . . ? N1A C1A C3A C4A 172(2) . . . . ? N2A C1A C3A C4A -5(3) . . . . ? N1A C1A C3A C21A -2(4) . . . . ? N2A C1A C3A C21A -179(2) . . . . ? C21A C3A C4A C5A 177(2) . . . . ? C1A C3A C4A C5A 2(3) . . . . ? C3A C4A C5A N2A 1(3) . . . . ? C3A C4A C5A C11A 176(2) . . . . ? C1A N2A C5A C4A -4(2) . . . . ? B1A N2A C5A C4A -173(2) . . . . ? C1A N2A C5A C11A -179(2) . . . . ? B1A N2A C5A C11A 12(4) . . . . ? C2A N3A C6A C7A 0(3) . . . . ? B1A N3A C6A C7A -177(2) . . . . ? C2A N3A C6A C31A 178(3) . . . . ? B1A N3A C6A C31A 1(5) . . . . ? N3A C6A C7A C8A 1(3) . . . . ? C31A C6A C7A C8A -178(2) . . . . ? N1A C2A C8A C41A -3(4) . . . . ? N3A C2A C8A C41A -178(2) . . . . ? N1A C2A C8A C7A 176(2) . . . . ? N3A C2A C8A C7A 1(2) . . . . ? C6A C7A C8A C2A -1(3) . . . . ? C6A C7A C8A C41A 179(2) . . . . ? C4A C5A C11A C16A -155(2) . . . . ? N2A C5A C11A C16A 19(4) . . . . ? C4A C5A C11A C12A 24(3) . . . . ? N2A C5A C11A C12A -162(2) . . . . ? C16A C11A C12A C13A 1(3) . . . . ? C5A C11A C12A C13A -178(2) . . . . ? C11A C12A C13A C14A -2(4) . . . . ? C12A C13A C14A C15A 6(4) . . . . ? C13A C14A C15A C16A -9(3) . . . . ? C14A C15A C16A C11A 8(3) . . . . ? C12A C11A C16A C15A -4(4) . . . . ? C5A C11A C16A C15A 175(2) . . . . ? C4A C3A C21A C22A 163(2) . . . . ? C1A C3A C21A C22A -24(4) . . . . ? C4A C3A C21A C26A -12(4) . . . . ? C1A C3A C21A C26A 162(2) . . . . ? C26A C21A C22A C23A -4(3) . . . . ? C3A C21A C22A C23A -178(2) . . . . ? C21A C22A C23A C24A 3(4) . . . . ? C22A C23A C24A N24A 175(2) . . . . ? C22A C23A C24A C25A 3(3) . . . . ? N24A C24A C25A C26A 179(3) . . . . ? C23A C24A C25A C26A -9(4) . . . . ? C24A C25A C26A C21A 9(4) . . . . ? C22A C21A C26A C25A -2(3) . . . . ? C3A C21A C26A C25A 172(2) . . . . ? C25A C24A N24A C28A -178(3) . . . . ? C23A C24A N24A C28A 10(4) . . . . ? C25A C24A N24A C27A -12(4) . . . . ? C23A C24A N24A C27A 176(2) . . . . ? N3A C6A C31A C32A 14(5) . . . . ? C7A C6A C31A C32A -169(2) . . . . ? N3A C6A C31A C36A -153(3) . . . . ? C7A C6A C31A C36A 25(4) . . . . ? C36A C31A C32A C33A -13(4) . . . . ? C6A C31A C32A C33A 180(3) . . . . ? C31A C32A C33A C34A 14(5) . . . . ? C32A C33A C34A C35A -10(5) . . . . ? C33A C34A C35A C36A 6(5) . . . . ? C34A C35A C36A C31A -7(5) . . . . ? C32A C31A C36A C35A 10(4) . . . . ? C6A C31A C36A C35A 177(3) . . . . ? C2A C8A C41A C42A 165(2) . . . . ? C7A C8A C41A C42A -15(4) . . . . ? C2A C8A C41A C46A -16(4) . . . . ? C7A C8A C41A C46A 164(2) . . . . ? C46A C41A C42A C43A 2(4) . . . . ? C8A C41A C42A C43A -178(2) . . . . ? C41A C42A C43A C44A -2(4) . . . . ? C42A C43A C44A N44A -180(2) . . . . ? C42A C43A C44A C45A 1(3) . . . . ? N44A C44A C45A C46A -180(3) . . . . ? C43A C44A C45A C46A 0(4) . . . . ? C44A C45A C46A C41A 1(4) . . . . ? C42A C41A C46A C45A -2(4) . . . . ? C8A C41A C46A C45A 179(2) . . . . ? C45A C44A N44A C47A 1(4) . . . . ? C43A C44A N44A C47A -179(2) . . . . ? C45A C44A N44A C48A 178(2) . . . . ? C43A C44A N44A C48A -2(3) . . . . ? C2B N1B C1B C3B -179(3) . . . . ? C2B N1B C1B N2B -3(4) . . . . ? N1B C1B N2B C5B -173(2) . . . . ? C3B C1B N2B C5B 3(2) . . . . ? N1B C1B N2B B1B 6(3) . . . . ? C3B C1B N2B B1B -177(2) . . . . ? C5B N2B B1B F1B -59(4) . . . . ? C1B N2B B1B F1B 122(2) . . . . ? C5B N2B B1B F2B 60(3) . . . . ? C1B N2B B1B F2B -120(2) . . . . ? C5B N2B B1B N3B 172(2) . . . . ? C1B N2B B1B N3B -7(3) . . . . ? F1B B1B N3B C6B 48(4) . . . . ? F2B B1B N3B C6B -76(3) . . . . ? N2B B1B N3B C6B 176(2) . . . . ? F1B B1B N3B C2B -121(3) . . . . ? F2B B1B N3B C2B 115(2) . . . . ? N2B B1B N3B C2B 7(3) . . . . ? C1B N1B C2B C8B -176(3) . . . . ? C1B N1B C2B N3B 2(4) . . . . ? C6B N3B C2B N1B -176(2) . . . . ? B1B N3B C2B N1B -4(4) . . . . ? C6B N3B C2B C8B 2(3) . . . . ? B1B N3B C2B C8B 174(2) . . . . ? N1B C1B C3B C4B 170(3) . . . . ? N2B C1B C3B C4B -6(3) . . . . ? N1B C1B C3B C21B 0(4) . . . . ? N2B C1B C3B C21B -176(2) . . . . ? C1B C3B C4B C5B 6(3) . . . . ? C21B C3B C4B C5B 175(2) . . . . ? C1B N2B C5B C4B 0(3) . . . . ? B1B N2B C5B C4B -179(2) . . . . ? C1B N2B C5B C11B 174(2) . . . . ? B1B N2B C5B C11B -6(4) . . . . ? C3B C4B C5B N2B -3(3) . . . . ? C3B C4B C5B C11B -177(2) . . . . ? C2B N3B C6B C7B -2(3) . . . . ? B1B N3B C6B C7B -172(2) . . . . ? C2B N3B C6B C31B 178(2) . . . . ? B1B N3B C6B C31B 7(4) . . . . ? N3B C6B C7B C8B 0(3) . . . . ? C31B C6B C7B C8B -179(2) . . . . ? N1B C2B C8B C41B -1(5) . . . . ? N3B C2B C8B C41B -179(2) . . . . ? N1B C2B C8B C7B 176(3) . . . . ? N3B C2B C8B C7B -2(3) . . . . ? C6B C7B C8B C41B 178(3) . . . . ? C6B C7B C8B C2B 1(3) . . . . ? N2B C5B C11B C12B -158(2) . . . . ? C4B C5B C11B C12B 15(3) . . . . ? N2B C5B C11B C16B 29(4) . . . . ? C4B C5B C11B C16B -158(2) . . . . ? C16B C11B C12B C13B -6(4) . . . . ? C5B C11B C12B C13B -178.7(19) . . . . ? C11B C12B C13B C14B 4(4) . . . . ? C12B C13B C14B C15B -2(4) . . . . ? C13B C14B C15B C16B 1(4) . . . . ? C12B C11B C16B C15B 5(4) . . . . ? C5B C11B C16B C15B 178(2) . . . . ? C14B C15B C16B C11B -3(4) . . . . ? C4B C3B C21B C22B 166(2) . . . . ? C1B C3B C21B C22B -26(4) . . . . ? C4B C3B C21B C26B -13(4) . . . . ? C1B C3B C21B C26B 155(2) . . . . ? C26B C21B C22B C23B -6(4) . . . . ? C3B C21B C22B C23B 175(2) . . . . ? C21B C22B C23B C24B 2(4) . . . . ? C22B C23B C24B N24B 180(3) . . . . ? C22B C23B C24B C25B 0(4) . . . . ? N24B C24B C25B C26B -178(3) . . . . ? C23B C24B C25B C26B 2(4) . . . . ? C24B C25B C26B C21B -6(4) . . . . ? C22B C21B C26B C25B 8(4) . . . . ? C3B C21B C26B C25B -173(2) . . . . ? C25B C24B N24B C28B -176(2) . . . . ? C23B C24B N24B C28B 5(4) . . . . ? C25B C24B N24B C27B 0(4) . . . . ? C23B C24B N24B C27B -179(2) . . . . ? C7B C6B C31B C36B 27(4) . . . . ? N3B C6B C31B C36B -153(2) . . . . ? C7B C6B C31B C32B -156(3) . . . . ? N3B C6B C31B C32B 25(4) . . . . ? C36B C31B C32B C33B 1(4) . . . . ? C6B C31B C32B C33B -176(3) . . . . ? C31B C32B C33B C34B -5(5) . . . . ? C32B C33B C34B C35B 6(5) . . . . ? C33B C34B C35B C36B -3(5) . . . . ? C34B C35B C36B C31B 0(4) . . . . ? C32B C31B C36B C35B 1(4) . . . . ? C6B C31B C36B C35B 179(2) . . . . ? C2B C8B C41B C42B 165(3) . . . . ? C7B C8B C41B C42B -11(4) . . . . ? C2B C8B C41B C46B -18(4) . . . . ? C7B C8B C41B C46B 166(2) . . . . ? C8B C41B C42B C43B -176(3) . . . . ? C46B C41B C42B C43B 6(4) . . . . ? C41B C42B C43B C44B -2(4) . . . . ? C42B C43B C44B N44B 178(2) . . . . ? C42B C43B C44B C45B -3(4) . . . . ? N44B C44B C45B C46B -178(2) . . . . ? C43B C44B C45B C46B 3(4) . . . . ? C44B C45B C46B C41B 2(4) . . . . ? C42B C41B C46B C45B -6(4) . . . . ? C8B C41B C46B C45B 176(2) . . . . ? C45B C44B N44B C48B -177(2) . . . . ? C43B C44B N44B C48B 2(4) . . . . ? C45B C44B N44B C47B 0(4) . . . . ? C43B C44B N44B C47B 179(2) . . . . ? _diffrn_measured_fraction_theta_max 0.98 _diffrn_reflns_theta_full 21.1 _diffrn_measured_fraction_theta_full 0.98 _refine_diff_density_max 0.30 _refine_diff_density_min -0.37 _refine_diff_density_rms 0.076 data_(Ib) _database_code_depnum_ccdc_archive 'CCDC 646559' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 532 _chemical_formula_moiety 'C36 H32 B F2 N5' _chemical_formula_sum 'C36 H32 B F2 N5' _chemical_formula_weight 583.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2169(7) _cell_length_b 14.0769(8) _cell_length_c 21.0039(15) _cell_angle_alpha 105.548(2) _cell_angle_beta 91.046(2) _cell_angle_gamma 92.138(5) _cell_volume 2907.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 59387 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.0 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.961 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'fine-focus sealed X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Kappa-CCD _diffrn_measurement_method '\f, \w scans with \k offsets' _diffrn_standards_number 59387 _diffrn_standards_decay_% ? _diffrn_reflns_number 27283 _diffrn_reflns_av_R_equivalents 0.1665 _diffrn_reflns_av_sigmaI/netI 0.2817 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 27.7 _diffrn_measured_fraction_theta_max 0.835 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.835 _reflns_number_total 11341 _reflns_number_gt 3569 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'kappaCCD Server software (Nonius, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (Burnett & Johnson) and PLATON (Spek, 2002)' _computing_publication_material 'SHELXL97 and PREP8 (Ferguson, 1998)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11341 _refine_ls_number_parameters 801 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2827 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2015 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.224 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.054 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1A F 0.2488(3) 0.1738(2) 0.23044(12) 0.0541(8) Uani 1 1 d . . . F2A F 0.4247(3) 0.2570(2) 0.20252(12) 0.0534(8) Uani 1 1 d . . . N1A N 0.3820(4) -0.0072(3) 0.07326(19) 0.0461(11) Uani 1 1 d . . . C1A C 0.4473(5) 0.0024(4) 0.1298(3) 0.0440(14) Uani 1 1 d . . . N2A N 0.4399(4) 0.0828(3) 0.1853(2) 0.0460(11) Uani 1 1 d . . . B1A B 0.3504(6) 0.1690(5) 0.1851(3) 0.0453(17) Uani 1 1 d . . . N3A N 0.2851(4) 0.1493(3) 0.11529(19) 0.0461(11) Uani 1 1 d . . . C2A C 0.3059(5) 0.0620(4) 0.0655(2) 0.0470(14) Uani 1 1 d . . . C3A C 0.5407(5) -0.0640(4) 0.1421(2) 0.0465(14) Uani 1 1 d . . . C4A C 0.5939(5) -0.0183(4) 0.2040(2) 0.0501(15) Uani 1 1 d . . . H4A H 0.6625 -0.0430 0.2253 0.060 Uiso 1 1 calc R . . C5A C 0.5327(5) 0.0691(4) 0.2305(3) 0.0505(15) Uani 1 1 d . . . C6A C 0.1901(5) 0.1983(4) 0.0904(3) 0.0471(14) Uani 1 1 d . . . C7A C 0.1553(5) 0.1427(4) 0.0265(2) 0.0519(15) Uani 1 1 d . . . H7A H 0.0923 0.1610 -0.0014 0.062 Uiso 1 1 calc R . . C8A C 0.2245(5) 0.0577(4) 0.0089(2) 0.0467(14) Uani 1 1 d . . . C11A C 0.5620(5) 0.1363(4) 0.2964(2) 0.0468(14) Uani 1 1 d . . . C12A C 0.6834(5) 0.1284(4) 0.3259(3) 0.0494(15) Uani 1 1 d . . . H12A H 0.7436 0.0826 0.3027 0.059 Uiso 1 1 calc R . . C13A C 0.7166(5) 0.1872(4) 0.3891(3) 0.0563(16) Uani 1 1 d . . . H13A H 0.8003 0.1830 0.4084 0.068 Uiso 1 1 calc R . . C14A C 0.6269(6) 0.2525(4) 0.4243(3) 0.0564(16) Uani 1 1 d . . . H14A H 0.6489 0.2919 0.4678 0.068 Uiso 1 1 calc R . . C15A C 0.5057(6) 0.2594(4) 0.3956(3) 0.0536(15) Uani 1 1 d . . . H15A H 0.4447 0.3038 0.4194 0.064 Uiso 1 1 calc R . . C16A C 0.4730(5) 0.2021(4) 0.3323(3) 0.0521(15) Uani 1 1 d . . . H16A H 0.3896 0.2073 0.3131 0.062 Uiso 1 1 calc R . . C21A C 0.5701(6) -0.1599(4) 0.0978(3) 0.0502(15) Uani 1 1 d . . . C22A C 0.4870(6) -0.2124(5) 0.0461(3) 0.0546(15) Uani 1 1 d . . . H22A H 0.4065 -0.1849 0.0386 0.065 Uiso 1 1 calc R . . C23A C 0.5166(6) -0.3020(5) 0.0058(3) 0.0607(17) Uani 1 1 d . . . H23A H 0.4580 -0.3342 -0.0297 0.073 Uiso 1 1 calc R . . C24A C 0.6319(6) -0.3471(5) 0.0160(3) 0.0557(16) Uani 1 1 d . . . C25A C 0.7156(6) -0.2957(5) 0.0677(3) 0.0549(16) Uani 1 1 d . . . H25A H 0.7957 -0.3234 0.0754 0.066 Uiso 1 1 calc R . . C26A C 0.6845(6) -0.2055(5) 0.1078(3) 0.0573(16) Uani 1 1 d . . . H26A H 0.7428 -0.1733 0.1434 0.069 Uiso 1 1 calc R . . C27A C 0.7872(6) -0.4793(5) -0.0185(3) 0.088(2) Uani 1 1 d . . . H27A H 0.8558 -0.4357 -0.0289 0.132 Uiso 1 1 calc R . . H27B H 0.7899 -0.5450 -0.0495 0.132 Uiso 1 1 calc R . . H27C H 0.8019 -0.4843 0.0267 0.132 Uiso 1 1 calc R . . N24A N 0.6599(5) -0.4390(4) -0.0240(2) 0.0736(15) Uani 1 1 d . . . C28A C 0.5813(6) -0.4842(5) -0.0840(3) 0.085(2) Uani 1 1 d . . . H28A H 0.4905 -0.4948 -0.0724 0.127 Uiso 1 1 calc R . . H28B H 0.6169 -0.5477 -0.1067 0.127 Uiso 1 1 calc R . . H28C H 0.5837 -0.4405 -0.1133 0.127 Uiso 1 1 calc R . . C31A C 0.1282(6) 0.2897(5) 0.1252(3) 0.0521(15) Uani 1 1 d . . . C32A C 0.1838(6) 0.3606(5) 0.1791(3) 0.0563(16) Uani 1 1 d . . . H32A H 0.2685 0.3517 0.1953 0.068 Uiso 1 1 calc R . . C33A C 0.1174(7) 0.4449(4) 0.2097(3) 0.0616(17) Uani 1 1 d . . . H33A H 0.1571 0.4918 0.2469 0.074 Uiso 1 1 calc R . . C34A C -0.0038(7) 0.4610(5) 0.1872(3) 0.0622(17) Uani 1 1 d . . . H34A H -0.0480 0.5191 0.2076 0.075 Uiso 1 1 calc R . . C35A C -0.0606(6) 0.3905(5) 0.1339(3) 0.0596(17) Uani 1 1 d . . . H35A H -0.1457 0.3994 0.1181 0.072 Uiso 1 1 calc R . . C36A C 0.0046(6) 0.3081(4) 0.1036(3) 0.0558(16) Uani 1 1 d . . . H36A H -0.0361 0.2618 0.0664 0.067 Uiso 1 1 calc R . . C41A C 0.2147(5) -0.0199(4) -0.0516(2) 0.0469(15) Uani 1 1 d . . . C42A C 0.1097(5) -0.0253(4) -0.0969(3) 0.0536(15) Uani 1 1 d . . . H42A H 0.0465 0.0240 -0.0868 0.064 Uiso 1 1 calc R . . C43A C 0.0943(5) -0.0987(5) -0.1552(3) 0.0551(16) Uani 1 1 d . . . H43A H 0.0205 -0.1000 -0.1836 0.066 Uiso 1 1 calc R . . C44A C 0.1865(5) -0.1715(4) -0.1728(3) 0.0473(14) Uani 1 1 d . . . C45A C 0.2915(5) -0.1677(4) -0.1278(2) 0.0499(15) Uani 1 1 d . . . H45A H 0.3548 -0.2169 -0.1377 0.060 Uiso 1 1 calc R . . C46A C 0.3038(5) -0.0945(4) -0.0701(3) 0.0507(15) Uani 1 1 d . . . H46A H 0.3764 -0.0942 -0.0412 0.061 Uiso 1 1 calc R . . C47A C 0.2633(5) -0.3214(4) -0.2511(2) 0.0598(17) Uani 1 1 d . . . H47A H 0.3533 -0.2938 -0.2417 0.090 Uiso 1 1 calc R . . H47B H 0.2514 -0.3527 -0.2986 0.090 Uiso 1 1 calc R . . H47C H 0.2469 -0.3707 -0.2266 0.090 Uiso 1 1 calc R . . N44A N 0.1722(4) -0.2430(4) -0.2311(2) 0.0540(12) Uani 1 1 d . . . C48A C 0.0579(5) -0.2478(4) -0.2750(2) 0.0575(16) Uani 1 1 d . . . H48A H -0.0222 -0.2527 -0.2509 0.086 Uiso 1 1 calc R . . H48B H 0.0617 -0.3059 -0.3130 0.086 Uiso 1 1 calc R . . H48C H 0.0577 -0.1880 -0.2905 0.086 Uiso 1 1 calc R . . F1B F 0.1005(3) 0.2771(2) 0.68740(12) 0.0558(8) Uani 1 1 d . . . F2B F 0.2357(3) 0.1983(2) 0.74294(12) 0.0553(8) Uani 1 1 d . . . N1B N 0.1365(4) 0.0052(3) 0.5752(2) 0.0490(12) Uani 1 1 d . . . C1B C 0.0501(5) 0.0198(4) 0.6241(2) 0.0466(14) Uani 1 1 d . . . N2B N 0.0579(4) 0.1027(3) 0.67910(19) 0.0452(11) Uani 1 1 d . . . B1B B 0.1593(6) 0.1885(6) 0.6858(3) 0.0516(18) Uani 1 1 d . . . N3B N 0.2474(4) 0.1614(3) 0.6238(2) 0.0477(12) Uani 1 1 d . . . C2B C 0.2283(5) 0.0712(4) 0.5754(2) 0.0456(14) Uani 1 1 d . . . C3B C -0.0479(5) -0.0503(4) 0.6315(2) 0.0444(14) Uani 1 1 d . . . C4B C -0.0981(5) -0.0079(4) 0.6934(2) 0.0448(14) Uani 1 1 d . . . H4B H -0.1656 -0.0370 0.7134 0.054 Uiso 1 1 calc R . . C5B C -0.0350(5) 0.0834(4) 0.7217(2) 0.0456(14) Uani 1 1 d . . . C6B C 0.3421(5) 0.2157(4) 0.6015(3) 0.0482(15) Uani 1 1 d . . . C7B C 0.3873(5) 0.1595(5) 0.5406(2) 0.0500(15) Uani 1 1 d . . . H7B H 0.4534 0.1808 0.5156 0.060 Uiso 1 1 calc R . . C8B C 0.3202(5) 0.0679(5) 0.5225(2) 0.0477(15) Uani 1 1 d . . . C11B C -0.0601(5) 0.1464(5) 0.7881(3) 0.0501(15) Uani 1 1 d . . . C12B C -0.1196(5) 0.1032(4) 0.8342(3) 0.0518(15) Uani 1 1 d . . . H12B H -0.1428 0.0346 0.8217 0.062 Uiso 1 1 calc R . . C13B C -0.1450(5) 0.1600(5) 0.8981(3) 0.0554(16) Uani 1 1 d . . . H13B H -0.1853 0.1299 0.9286 0.066 Uiso 1 1 calc R . . C14B C -0.1122(5) 0.2578(5) 0.9163(3) 0.0583(16) Uani 1 1 d . . . H14B H -0.1288 0.2959 0.9598 0.070 Uiso 1 1 calc R . . C15B C -0.0548(5) 0.3026(4) 0.8722(3) 0.0543(15) Uani 1 1 d . . . H15B H -0.0343 0.3716 0.8850 0.065 Uiso 1 1 calc R . . C16B C -0.0271(5) 0.2473(5) 0.8096(2) 0.0549(16) Uani 1 1 d . . . H16B H 0.0154 0.2785 0.7802 0.066 Uiso 1 1 calc R . . C21B C -0.0786(5) -0.1461(4) 0.5856(3) 0.0464(14) Uani 1 1 d . . . C22B C -0.0441(5) -0.1699(4) 0.5184(3) 0.0495(15) Uani 1 1 d . . . H22B H -0.0065 -0.1195 0.5013 0.059 Uiso 1 1 calc R . . C23B C -0.0628(5) -0.2634(4) 0.4770(3) 0.0522(15) Uani 1 1 d . . . H23B H -0.0398 -0.2753 0.4320 0.063 Uiso 1 1 calc R . . C24B C -0.1156(5) -0.3420(5) 0.4996(3) 0.0514(15) Uani 1 1 d . . . C25B C -0.1544(5) -0.3161(5) 0.5662(3) 0.0532(15) Uani 1 1 d . . . H25B H -0.1951 -0.3657 0.5832 0.064 Uiso 1 1 calc R . . C26B C -0.1359(5) -0.2234(4) 0.6070(3) 0.0505(15) Uani 1 1 d . . . H26B H -0.1628 -0.2108 0.6514 0.061 Uiso 1 1 calc R . . C27B C -0.1899(5) -0.5136(4) 0.4815(3) 0.0683(17) Uani 1 1 d . . . H27D H -0.1906 -0.5751 0.4459 0.102 Uiso 1 1 calc R . . H27E H -0.2802 -0.4963 0.4928 0.102 Uiso 1 1 calc R . . H27F H -0.1428 -0.5225 0.5204 0.102 Uiso 1 1 calc R . . N24B N -0.1250(4) -0.4352(4) 0.4597(2) 0.0628(13) Uani 1 1 d . . . C28B C -0.0881(6) -0.4565(5) 0.3908(3) 0.0736(18) Uani 1 1 d . . . H28D H 0.0006 -0.4290 0.3884 0.110 Uiso 1 1 calc R . . H28E H -0.1498 -0.4268 0.3663 0.110 Uiso 1 1 calc R . . H28F H -0.0902 -0.5281 0.3715 0.110 Uiso 1 1 calc R . . C31B C 0.3887(5) 0.3171(4) 0.6335(3) 0.0497(15) Uani 1 1 d . . . C32B C 0.3888(5) 0.3612(4) 0.7020(3) 0.0508(15) Uani 1 1 d . . . H32B H 0.3547 0.3253 0.7308 0.061 Uiso 1 1 calc R . . C33B C 0.4382(5) 0.4561(5) 0.7272(3) 0.0561(16) Uani 1 1 d . . . H33B H 0.4377 0.4847 0.7736 0.067 Uiso 1 1 calc R . . C34B C 0.4888(5) 0.5117(5) 0.6873(3) 0.0604(16) Uani 1 1 d . . . H34B H 0.5222 0.5775 0.7059 0.072 Uiso 1 1 calc R . . C35B C 0.4895(5) 0.4695(4) 0.6203(3) 0.0562(16) Uani 1 1 d . . . H35B H 0.5238 0.5062 0.5920 0.067 Uiso 1 1 calc R . . C36B C 0.4413(5) 0.3752(4) 0.5941(3) 0.0556(16) Uani 1 1 d . . . H36B H 0.4431 0.3476 0.5476 0.067 Uiso 1 1 calc R . . C41B C 0.3302(5) -0.0109(4) 0.4629(2) 0.0456(14) Uani 1 1 d . . . C42B C 0.4007(5) 0.0036(4) 0.4091(2) 0.0472(14) Uani 1 1 d . . . H42B H 0.4467 0.0650 0.4134 0.057 Uiso 1 1 calc R . . C43B C 0.4043(5) -0.0689(4) 0.3506(2) 0.0482(14) Uani 1 1 d . . . H43B H 0.4519 -0.0562 0.3151 0.058 Uiso 1 1 calc R . . C44B C 0.3400(5) -0.1606(5) 0.3422(3) 0.0486(14) Uani 1 1 d . . . C45B C 0.2735(5) -0.1774(4) 0.3968(2) 0.0530(15) Uani 1 1 d . . . H45B H 0.2304 -0.2397 0.3932 0.064 Uiso 1 1 calc R . . C46B C 0.2708(5) -0.1047(5) 0.4546(3) 0.0528(15) Uani 1 1 d . . . H46B H 0.2266 -0.1184 0.4907 0.063 Uiso 1 1 calc R . . C47B C 0.2731(5) -0.3261(4) 0.2762(2) 0.0574(16) Uani 1 1 d . . . H47D H 0.1798 -0.3170 0.2846 0.086 Uiso 1 1 calc R . . H47E H 0.3111 -0.3579 0.3080 0.086 Uiso 1 1 calc R . . H47F H 0.2835 -0.3678 0.2312 0.086 Uiso 1 1 calc R . . N44B N 0.3385(4) -0.2326(3) 0.2833(2) 0.0509(12) Uani 1 1 d . . . C48B C 0.4054(5) -0.2144(4) 0.2268(2) 0.0621(17) Uani 1 1 d . . . H48D H 0.4989 -0.1999 0.2381 0.093 Uiso 1 1 calc R . . H48E H 0.3678 -0.1580 0.2153 0.093 Uiso 1 1 calc R . . H48F H 0.3947 -0.2730 0.1891 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1A 0.0641(19) 0.066(2) 0.0335(17) 0.0133(16) 0.0096(15) 0.0121(17) F2A 0.069(2) 0.053(2) 0.0356(18) 0.0077(16) 0.0022(15) 0.0017(18) N1A 0.058(3) 0.052(3) 0.028(3) 0.011(2) 0.004(2) 0.003(3) C1A 0.048(4) 0.048(4) 0.036(3) 0.011(3) 0.004(3) 0.001(3) N2A 0.055(3) 0.048(3) 0.035(3) 0.011(3) 0.006(2) 0.004(2) B1A 0.046(4) 0.053(5) 0.033(4) 0.006(3) 0.004(3) -0.001(4) N3A 0.061(3) 0.051(3) 0.028(3) 0.013(2) 0.007(2) 0.006(3) C2A 0.055(4) 0.054(4) 0.031(3) 0.009(3) 0.005(3) 0.011(3) C3A 0.060(4) 0.055(4) 0.026(3) 0.012(3) 0.006(3) 0.002(3) C4A 0.061(4) 0.059(4) 0.035(3) 0.019(3) 0.009(3) 0.014(3) C5A 0.057(4) 0.056(4) 0.041(4) 0.017(3) 0.005(3) 0.001(3) C6A 0.063(4) 0.049(4) 0.035(3) 0.020(3) 0.006(3) 0.001(3) C7A 0.063(4) 0.062(4) 0.031(3) 0.012(3) 0.002(3) 0.010(3) C8A 0.056(4) 0.052(4) 0.033(3) 0.012(3) 0.001(3) 0.001(3) C11A 0.061(4) 0.054(4) 0.032(3) 0.020(3) 0.005(3) 0.005(3) C12A 0.061(4) 0.056(4) 0.039(3) 0.024(3) 0.004(3) 0.007(3) C13A 0.067(4) 0.073(5) 0.032(3) 0.019(3) 0.001(3) 0.003(4) C14A 0.070(4) 0.064(4) 0.034(3) 0.013(3) 0.006(3) -0.002(4) C15A 0.057(4) 0.064(4) 0.043(4) 0.018(3) 0.005(3) 0.006(3) C16A 0.064(4) 0.061(4) 0.038(3) 0.025(3) 0.008(3) 0.006(3) C21A 0.064(4) 0.058(4) 0.032(3) 0.018(3) 0.004(3) 0.010(4) C22A 0.065(4) 0.060(5) 0.038(3) 0.010(3) 0.005(3) 0.008(3) C23A 0.078(5) 0.059(5) 0.037(4) -0.001(3) -0.003(3) 0.008(4) C24A 0.077(5) 0.044(4) 0.044(4) 0.004(3) 0.017(3) 0.016(4) C25A 0.065(4) 0.066(5) 0.036(3) 0.017(3) 0.005(3) 0.012(4) C26A 0.080(5) 0.059(4) 0.036(3) 0.016(3) 0.013(3) 0.015(4) C27A 0.105(6) 0.081(5) 0.081(5) 0.017(4) 0.027(4) 0.040(5) N24A 0.095(4) 0.070(4) 0.056(4) 0.016(3) 0.019(3) 0.019(4) C28A 0.113(5) 0.072(5) 0.057(4) -0.005(4) 0.015(4) 0.001(4) C31A 0.057(4) 0.067(5) 0.040(4) 0.024(4) 0.010(3) 0.017(4) C32A 0.061(4) 0.060(5) 0.049(4) 0.017(4) 0.009(3) 0.002(4) C33A 0.085(5) 0.049(4) 0.049(4) 0.009(3) 0.012(4) 0.012(4) C34A 0.083(5) 0.049(4) 0.055(4) 0.013(4) 0.013(4) 0.009(4) C35A 0.071(4) 0.065(5) 0.047(4) 0.021(4) 0.009(3) 0.021(4) C36A 0.067(4) 0.064(5) 0.039(3) 0.017(3) 0.012(3) 0.013(4) C41A 0.052(4) 0.061(4) 0.028(3) 0.012(3) 0.012(3) 0.012(3) C42A 0.064(4) 0.061(4) 0.039(4) 0.019(3) 0.000(3) 0.011(3) C43A 0.057(4) 0.069(5) 0.037(4) 0.009(3) 0.004(3) 0.010(4) C44A 0.058(4) 0.058(4) 0.030(3) 0.018(3) 0.009(3) -0.003(3) C45A 0.059(4) 0.060(4) 0.031(3) 0.012(3) 0.007(3) 0.008(3) C46A 0.055(4) 0.068(4) 0.035(3) 0.023(3) 0.008(3) 0.007(3) C47A 0.075(4) 0.065(4) 0.037(3) 0.007(3) 0.008(3) 0.013(4) N44A 0.060(3) 0.064(4) 0.038(3) 0.014(3) 0.001(3) 0.009(3) C48A 0.069(4) 0.069(4) 0.031(3) 0.008(3) 0.000(3) 0.002(3) F1B 0.074(2) 0.057(2) 0.0385(18) 0.0157(16) 0.0109(15) 0.0123(18) F2B 0.0666(19) 0.066(2) 0.0325(17) 0.0136(16) -0.0005(15) -0.0020(17) N1B 0.052(3) 0.060(3) 0.037(3) 0.016(2) 0.005(2) 0.002(3) C1B 0.061(4) 0.054(4) 0.028(3) 0.014(3) 0.006(3) 0.010(3) N2B 0.051(3) 0.060(3) 0.025(2) 0.012(2) 0.002(2) 0.011(3) B1B 0.054(4) 0.065(6) 0.037(4) 0.016(4) -0.001(3) -0.002(4) N3B 0.055(3) 0.050(3) 0.038(3) 0.012(3) 0.004(2) 0.003(3) C2B 0.055(4) 0.048(4) 0.034(3) 0.012(3) -0.002(3) 0.001(3) C3B 0.049(3) 0.051(4) 0.041(3) 0.024(3) 0.006(3) 0.005(3) C4B 0.045(3) 0.054(4) 0.036(3) 0.013(3) 0.008(3) 0.001(3) C5B 0.045(3) 0.060(4) 0.036(3) 0.020(3) 0.000(3) 0.007(3) C6B 0.050(4) 0.057(4) 0.044(4) 0.024(3) -0.004(3) 0.003(3) C7B 0.060(4) 0.063(5) 0.029(3) 0.014(3) 0.008(3) 0.013(3) C8B 0.059(4) 0.054(4) 0.032(3) 0.015(3) 0.001(3) 0.006(3) C11B 0.056(4) 0.060(5) 0.034(3) 0.010(3) 0.001(3) 0.006(3) C12B 0.063(4) 0.053(4) 0.044(4) 0.018(3) 0.012(3) 0.014(3) C13B 0.060(4) 0.066(5) 0.043(4) 0.017(4) 0.012(3) 0.008(4) C14B 0.072(4) 0.065(5) 0.035(3) 0.007(3) 0.005(3) 0.004(4) C15B 0.062(4) 0.055(4) 0.047(4) 0.016(3) 0.009(3) 0.004(3) C16B 0.069(4) 0.065(5) 0.032(3) 0.015(3) 0.016(3) 0.007(4) C21B 0.057(4) 0.044(4) 0.040(3) 0.014(3) 0.004(3) 0.003(3) C22B 0.050(3) 0.056(4) 0.046(4) 0.021(3) 0.006(3) 0.001(3) C23B 0.069(4) 0.048(4) 0.038(3) 0.008(3) -0.001(3) 0.002(3) C24B 0.063(4) 0.049(4) 0.042(4) 0.011(3) -0.005(3) -0.003(3) C25B 0.052(4) 0.067(5) 0.041(4) 0.018(3) -0.002(3) -0.004(3) C26B 0.061(4) 0.055(4) 0.035(3) 0.011(3) -0.002(3) -0.005(3) C27B 0.090(4) 0.049(4) 0.066(4) 0.017(3) -0.003(3) -0.009(4) N24B 0.091(4) 0.049(4) 0.044(3) 0.007(3) -0.003(3) -0.012(3) C28B 0.100(5) 0.063(5) 0.050(4) 0.003(3) 0.005(3) 0.002(4) C31B 0.049(4) 0.050(4) 0.052(4) 0.018(3) 0.002(3) 0.005(3) C32B 0.065(4) 0.053(4) 0.035(3) 0.012(3) 0.004(3) 0.001(3) C33B 0.064(4) 0.061(5) 0.035(3) -0.002(3) 0.005(3) 0.005(4) C34B 0.072(4) 0.052(4) 0.050(4) 0.000(3) 0.009(3) 0.005(3) C35B 0.071(4) 0.040(4) 0.054(4) 0.009(3) 0.005(3) -0.011(3) C36B 0.077(4) 0.054(4) 0.037(3) 0.015(3) 0.011(3) 0.003(4) C41B 0.056(4) 0.050(4) 0.031(3) 0.011(3) 0.005(3) 0.007(3) C42B 0.062(4) 0.043(4) 0.039(3) 0.015(3) 0.006(3) 0.003(3) C43B 0.061(4) 0.050(4) 0.034(3) 0.013(3) 0.005(3) -0.001(3) C44B 0.055(4) 0.055(4) 0.034(3) 0.008(3) -0.005(3) 0.003(3) C45B 0.068(4) 0.060(4) 0.033(3) 0.015(3) 0.010(3) 0.002(3) C46B 0.062(4) 0.062(5) 0.038(4) 0.016(3) 0.009(3) 0.012(3) C47B 0.072(4) 0.057(4) 0.039(3) 0.008(3) 0.009(3) -0.008(3) N44B 0.065(3) 0.052(3) 0.032(3) 0.006(3) 0.003(2) -0.008(3) C48B 0.076(4) 0.068(5) 0.039(3) 0.010(3) 0.015(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1A B1A 1.413(6) . ? F2A B1A 1.386(7) . ? N1A C2A 1.310(6) . ? N1A C1A 1.323(6) . ? C1A N2A 1.395(6) . ? C1A C3A 1.429(7) . ? N2A C5A 1.384(6) . ? N2A B1A 1.548(7) . ? B1A N3A 1.550(7) . ? N3A C6A 1.384(6) . ? N3A C2A 1.410(6) . ? C2A C8A 1.425(6) . ? C3A C4A 1.377(7) . ? C3A C21A 1.466(7) . ? C4A C5A 1.385(7) . ? C4A H4A 0.9500 . ? C5A C11A 1.470(7) . ? C6A C7A 1.392(7) . ? C6A C31A 1.470(7) . ? C7A C8A 1.380(7) . ? C7A H7A 0.9500 . ? C8A C41A 1.437(7) . ? C11A C12A 1.398(6) . ? C11A C16A 1.403(6) . ? C12A C13A 1.392(7) . ? C12A H12A 0.9500 . ? C13A C14A 1.398(7) . ? C13A H13A 0.9500 . ? C14A C15A 1.386(7) . ? C14A H14A 0.9500 . ? C15A C16A 1.385(7) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C21A C22A 1.390(7) . ? C21A C26A 1.394(7) . ? C22A C23A 1.365(7) . ? C22A H22A 0.9500 . ? C23A C24A 1.399(7) . ? C23A H23A 0.9500 . ? C24A N24A 1.384(7) . ? C24A C25A 1.389(7) . ? C25A C26A 1.374(7) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? C27A N24A 1.454(6) . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? N24A C28A 1.461(7) . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C31A C32A 1.388(7) . ? C31A C36A 1.392(7) . ? C32A C33A 1.396(7) . ? C32A H32A 0.9500 . ? C33A C34A 1.366(7) . ? C33A H33A 0.9500 . ? C34A C35A 1.383(8) . ? C34A H34A 0.9500 . ? C35A C36A 1.367(7) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? C41A C46A 1.395(6) . ? C41A C42A 1.408(6) . ? C42A C43A 1.376(7) . ? C42A H42A 0.9500 . ? C43A C44A 1.398(7) . ? C43A H43A 0.9500 . ? C44A N44A 1.361(6) . ? C44A C45A 1.407(6) . ? C45A C46A 1.365(7) . ? C45A H45A 0.9500 . ? C46A H46A 0.9500 . ? C47A N44A 1.451(6) . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? N44A C48A 1.463(6) . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? F1B B1B 1.397(7) . ? F2B B1B 1.392(6) . ? N1B C2B 1.294(6) . ? N1B C1B 1.346(6) . ? C1B N2B 1.403(6) . ? C1B C3B 1.419(7) . ? N2B C5B 1.386(6) . ? N2B B1B 1.538(8) . ? B1B N3B 1.566(7) . ? N3B C6B 1.377(6) . ? N3B C2B 1.402(6) . ? C2B C8B 1.460(6) . ? C3B C4B 1.393(6) . ? C3B C21B 1.452(7) . ? C4B C5B 1.390(7) . ? C4B H4B 0.9500 . ? C5B C11B 1.471(7) . ? C6B C7B 1.408(7) . ? C6B C31B 1.462(7) . ? C7B C8B 1.393(7) . ? C7B H7B 0.9500 . ? C8B C41B 1.441(7) . ? C11B C16B 1.395(7) . ? C11B C12B 1.409(6) . ? C12B C13B 1.400(7) . ? C12B H12B 0.9500 . ? C13B C14B 1.353(7) . ? C13B H13B 0.9500 . ? C14B C15B 1.380(6) . ? C14B H14B 0.9500 . ? C15B C16B 1.377(7) . ? C15B H15B 0.9500 . ? C16B H16B 0.9500 . ? C21B C26B 1.399(7) . ? C21B C22B 1.414(6) . ? C22B C23B 1.373(7) . ? C22B H22B 0.9500 . ? C23B C24B 1.411(7) . ? C23B H23B 0.9500 . ? C24B N24B 1.353(7) . ? C24B C25B 1.416(6) . ? C25B C26B 1.360(7) . ? C25B H25B 0.9500 . ? C26B H26B 0.9500 . ? C27B N24B 1.447(6) . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? N24B C28B 1.456(6) . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C31B C32B 1.406(7) . ? C31B C36B 1.410(7) . ? C32B C33B 1.372(7) . ? C32B H32B 0.9500 . ? C33B C34B 1.385(7) . ? C33B H33B 0.9500 . ? C34B C35B 1.375(7) . ? C34B H34B 0.9500 . ? C35B C36B 1.363(7) . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? C41B C46B 1.397(7) . ? C41B C42B 1.408(6) . ? C42B C43B 1.373(7) . ? C42B H42B 0.9500 . ? C43B C44B 1.392(7) . ? C43B H43B 0.9500 . ? C44B N44B 1.373(6) . ? C44B C45B 1.412(6) . ? C45B C46B 1.363(7) . ? C45B H45B 0.9500 . ? C46B H46B 0.9500 . ? C47B N44B 1.423(6) . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? N44B C48B 1.456(5) . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A N1A C1A 120.7(5) . . ? N1A C1A N2A 124.5(5) . . ? N1A C1A C3A 125.6(5) . . ? N2A C1A C3A 109.8(5) . . ? C5A N2A C1A 106.0(4) . . ? C5A N2A B1A 132.5(5) . . ? C1A N2A B1A 121.2(4) . . ? F2A B1A F1A 109.0(5) . . ? F2A B1A N2A 109.1(4) . . ? F1A B1A N2A 110.9(5) . . ? F2A B1A N3A 112.1(5) . . ? F1A B1A N3A 107.3(4) . . ? N2A B1A N3A 108.3(4) . . ? C6A N3A C2A 106.5(4) . . ? C6A N3A B1A 131.8(4) . . ? C2A N3A B1A 121.3(4) . . ? N1A C2A N3A 123.9(5) . . ? N1A C2A C8A 126.0(5) . . ? N3A C2A C8A 109.8(5) . . ? C4A C3A C1A 104.9(5) . . ? C4A C3A C21A 128.7(5) . . ? C1A C3A C21A 126.4(5) . . ? C3A C4A C5A 109.9(5) . . ? C3A C4A H4A 125.0 . . ? C5A C4A H4A 125.0 . . ? N2A C5A C4A 109.2(5) . . ? N2A C5A C11A 125.7(5) . . ? C4A C5A C11A 125.1(5) . . ? N3A C6A C7A 108.1(5) . . ? N3A C6A C31A 127.2(5) . . ? C7A C6A C31A 124.5(5) . . ? C8A C7A C6A 111.1(5) . . ? C8A C7A H7A 124.5 . . ? C6A C7A H7A 124.5 . . ? C7A C8A C2A 104.5(5) . . ? C7A C8A C41A 128.3(5) . . ? C2A C8A C41A 127.2(5) . . ? C12A C11A C16A 118.9(5) . . ? C12A C11A C5A 117.0(5) . . ? C16A C11A C5A 124.0(5) . . ? C13A C12A C11A 120.3(5) . . ? C13A C12A H12A 119.8 . . ? C11A C12A H12A 119.8 . . ? C12A C13A C14A 120.1(5) . . ? C12A C13A H13A 120.0 . . ? C14A C13A H13A 120.0 . . ? C15A C14A C13A 119.7(5) . . ? C15A C14A H14A 120.1 . . ? C13A C14A H14A 120.1 . . ? C16A C15A C14A 120.4(5) . . ? C16A C15A H15A 119.8 . . ? C14A C15A H15A 119.8 . . ? C15A C16A C11A 120.5(5) . . ? C15A C16A H16A 119.7 . . ? C11A C16A H16A 119.7 . . ? C22A C21A C26A 116.1(5) . . ? C22A C21A C3A 123.8(5) . . ? C26A C21A C3A 120.1(5) . . ? C23A C22A C21A 122.5(5) . . ? C23A C22A H22A 118.7 . . ? C21A C22A H22A 118.7 . . ? C22A C23A C24A 121.0(6) . . ? C22A C23A H23A 119.5 . . ? C24A C23A H23A 119.5 . . ? N24A C24A C25A 122.2(6) . . ? N24A C24A C23A 120.7(6) . . ? C25A C24A C23A 117.1(5) . . ? C26A C25A C24A 121.2(5) . . ? C26A C25A H25A 119.4 . . ? C24A C25A H25A 119.4 . . ? C25A C26A C21A 122.0(6) . . ? C25A C26A H26A 119.0 . . ? C21A C26A H26A 119.0 . . ? N24A C27A H27A 109.5 . . ? N24A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? N24A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C24A N24A C27A 120.1(6) . . ? C24A N24A C28A 120.8(5) . . ? C27A N24A C28A 116.7(5) . . ? N24A C28A H28A 109.5 . . ? N24A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? N24A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C32A C31A C36A 116.3(5) . . ? C32A C31A C6A 125.0(5) . . ? C36A C31A C6A 118.8(6) . . ? C31A C32A C33A 121.2(5) . . ? C31A C32A H32A 119.4 . . ? C33A C32A H32A 119.4 . . ? C34A C33A C32A 121.0(6) . . ? C34A C33A H33A 119.5 . . ? C32A C33A H33A 119.5 . . ? C33A C34A C35A 118.3(6) . . ? C33A C34A H34A 120.9 . . ? C35A C34A H34A 120.9 . . ? C36A C35A C34A 120.7(6) . . ? C36A C35A H35A 119.6 . . ? C34A C35A H35A 119.6 . . ? C35A C36A C31A 122.5(6) . . ? C35A C36A H36A 118.8 . . ? C31A C36A H36A 118.8 . . ? C46A C41A C42A 115.2(5) . . ? C46A C41A C8A 124.4(5) . . ? C42A C41A C8A 120.5(5) . . ? C43A C42A C41A 123.0(5) . . ? C43A C42A H42A 118.5 . . ? C41A C42A H42A 118.5 . . ? C42A C43A C44A 120.5(5) . . ? C42A C43A H43A 119.8 . . ? C44A C43A H43A 119.8 . . ? N44A C44A C43A 120.3(5) . . ? N44A C44A C45A 122.4(5) . . ? C43A C44A C45A 117.3(5) . . ? C46A C45A C44A 121.0(5) . . ? C46A C45A H45A 119.5 . . ? C44A C45A H45A 119.5 . . ? C45A C46A C41A 123.1(5) . . ? C45A C46A H46A 118.4 . . ? C41A C46A H46A 118.4 . . ? N44A C47A H47A 109.5 . . ? N44A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? N44A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C44A N44A C47A 122.6(5) . . ? C44A N44A C48A 120.9(5) . . ? C47A N44A C48A 116.4(4) . . ? N44A C48A H48A 109.5 . . ? N44A C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? N44A C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C2B N1B C1B 120.5(5) . . ? N1B C1B N2B 122.9(5) . . ? N1B C1B C3B 125.2(5) . . ? N2B C1B C3B 111.4(4) . . ? C5B N2B C1B 105.1(5) . . ? C5B N2B B1B 132.1(5) . . ? C1B N2B B1B 122.7(4) . . ? F2B B1B F1B 110.4(5) . . ? F2B B1B N2B 108.6(5) . . ? F1B B1B N2B 112.2(5) . . ? F2B B1B N3B 109.8(5) . . ? F1B B1B N3B 108.3(5) . . ? N2B B1B N3B 107.4(5) . . ? C6B N3B C2B 107.1(4) . . ? C6B N3B B1B 131.5(5) . . ? C2B N3B B1B 121.2(5) . . ? N1B C2B N3B 125.1(5) . . ? N1B C2B C8B 125.5(5) . . ? N3B C2B C8B 109.2(5) . . ? C4B C3B C1B 103.9(5) . . ? C4B C3B C21B 129.8(5) . . ? C1B C3B C21B 126.2(5) . . ? C5B C4B C3B 110.1(5) . . ? C5B C4B H4B 124.9 . . ? C3B C4B H4B 124.9 . . ? N2B C5B C4B 109.5(5) . . ? N2B C5B C11B 125.9(5) . . ? C4B C5B C11B 124.6(5) . . ? N3B C6B C7B 109.5(5) . . ? N3B C6B C31B 126.8(5) . . ? C7B C6B C31B 123.7(5) . . ? C8B C7B C6B 109.5(5) . . ? C8B C7B H7B 125.2 . . ? C6B C7B H7B 125.2 . . ? C7B C8B C41B 128.6(5) . . ? C7B C8B C2B 104.7(5) . . ? C41B C8B C2B 126.6(6) . . ? C16B C11B C12B 116.9(5) . . ? C16B C11B C5B 124.4(5) . . ? C12B C11B C5B 118.7(5) . . ? C13B C12B C11B 120.9(5) . . ? C13B C12B H12B 119.6 . . ? C11B C12B H12B 119.6 . . ? C14B C13B C12B 120.0(5) . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C13B C14B C15B 120.6(5) . . ? C13B C14B H14B 119.7 . . ? C15B C14B H14B 119.7 . . ? C16B C15B C14B 120.0(6) . . ? C16B C15B H15B 120.0 . . ? C14B C15B H15B 120.0 . . ? C15B C16B C11B 121.6(5) . . ? C15B C16B H16B 119.2 . . ? C11B C16B H16B 119.2 . . ? C26B C21B C22B 115.7(5) . . ? C26B C21B C3B 121.1(5) . . ? C22B C21B C3B 123.0(5) . . ? C23B C22B C21B 122.5(5) . . ? C23B C22B H22B 118.8 . . ? C21B C22B H22B 118.8 . . ? C22B C23B C24B 121.6(5) . . ? C22B C23B H23B 119.2 . . ? C24B C23B H23B 119.2 . . ? N24B C24B C23B 121.1(5) . . ? N24B C24B C25B 123.6(5) . . ? C23B C24B C25B 115.3(6) . . ? C26B C25B C24B 122.8(5) . . ? C26B C25B H25B 118.6 . . ? C24B C25B H25B 118.6 . . ? C25B C26B C21B 122.1(5) . . ? C25B C26B H26B 118.9 . . ? C21B C26B H26B 118.9 . . ? N24B C27B H27D 109.5 . . ? N24B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? N24B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C24B N24B C27B 120.5(5) . . ? C24B N24B C28B 121.0(5) . . ? C27B N24B C28B 117.8(5) . . ? N24B C28B H28D 109.5 . . ? N24B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? N24B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C32B C31B C36B 116.5(5) . . ? C32B C31B C6B 124.7(5) . . ? C36B C31B C6B 118.8(5) . . ? C33B C32B C31B 120.0(5) . . ? C33B C32B H32B 120.0 . . ? C31B C32B H32B 120.0 . . ? C32B C33B C34B 122.3(5) . . ? C32B C33B H33B 118.8 . . ? C34B C33B H33B 118.8 . . ? C35B C34B C33B 118.3(6) . . ? C35B C34B H34B 120.8 . . ? C33B C34B H34B 120.8 . . ? C36B C35B C34B 120.4(5) . . ? C36B C35B H35B 119.8 . . ? C34B C35B H35B 119.8 . . ? C35B C36B C31B 122.4(5) . . ? C35B C36B H36B 118.8 . . ? C31B C36B H36B 118.8 . . ? C46B C41B C42B 116.2(5) . . ? C46B C41B C8B 122.9(5) . . ? C42B C41B C8B 120.8(5) . . ? C43B C42B C41B 121.4(5) . . ? C43B C42B H42B 119.3 . . ? C41B C42B H42B 119.3 . . ? C42B C43B C44B 121.5(5) . . ? C42B C43B H43B 119.2 . . ? C44B C43B H43B 119.2 . . ? N44B C44B C43B 122.3(5) . . ? N44B C44B C45B 120.2(6) . . ? C43B C44B C45B 117.5(5) . . ? C46B C45B C44B 120.3(6) . . ? C46B C45B H45B 119.8 . . ? C44B C45B H45B 119.8 . . ? C45B C46B C41B 122.9(5) . . ? C45B C46B H46B 118.5 . . ? C41B C46B H46B 118.5 . . ? N44B C47B H47D 109.5 . . ? N44B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? N44B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C44B N44B C47B 121.2(5) . . ? C44B N44B C48B 120.0(5) . . ? C47B N44B C48B 118.8(4) . . ? N44B C48B H48D 109.5 . . ? N44B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? N44B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A N1A C1A N2A 1.5(8) . . . . ? C2A N1A C1A C3A -174.7(5) . . . . ? N1A C1A N2A C5A -173.7(5) . . . . ? C3A C1A N2A C5A 3.0(5) . . . . ? N1A C1A N2A B1A 0.8(7) . . . . ? C3A C1A N2A B1A 177.5(4) . . . . ? C5A N2A B1A F2A 47.6(7) . . . . ? C1A N2A B1A F2A -125.2(5) . . . . ? C5A N2A B1A F1A -72.6(7) . . . . ? C1A N2A B1A F1A 114.7(5) . . . . ? C5A N2A B1A N3A 170.0(5) . . . . ? C1A N2A B1A N3A -2.8(6) . . . . ? F2A B1A N3A C6A -65.4(7) . . . . ? F1A B1A N3A C6A 54.3(7) . . . . ? N2A B1A N3A C6A 174.1(4) . . . . ? F2A B1A N3A C2A 123.6(5) . . . . ? F1A B1A N3A C2A -116.7(5) . . . . ? N2A B1A N3A C2A 3.1(7) . . . . ? C1A N1A C2A N3A -1.2(8) . . . . ? C1A N1A C2A C8A -175.7(5) . . . . ? C6A N3A C2A N1A -174.4(5) . . . . ? B1A N3A C2A N1A -1.4(8) . . . . ? C6A N3A C2A C8A 0.9(5) . . . . ? B1A N3A C2A C8A 173.9(4) . . . . ? N1A C1A C3A C4A 172.9(5) . . . . ? N2A C1A C3A C4A -3.8(6) . . . . ? N1A C1A C3A C21A -7.6(8) . . . . ? N2A C1A C3A C21A 175.7(5) . . . . ? C1A C3A C4A C5A 3.1(6) . . . . ? C21A C3A C4A C5A -176.4(5) . . . . ? C1A N2A C5A C4A -1.1(5) . . . . ? B1A N2A C5A C4A -174.6(5) . . . . ? C1A N2A C5A C11A 179.1(5) . . . . ? B1A N2A C5A C11A 5.5(8) . . . . ? C3A C4A C5A N2A -1.3(6) . . . . ? C3A C4A C5A C11A 178.5(5) . . . . ? C2A N3A C6A C7A -0.9(5) . . . . ? B1A N3A C6A C7A -172.9(5) . . . . ? C2A N3A C6A C31A 175.5(5) . . . . ? B1A N3A C6A C31A 3.5(8) . . . . ? N3A C6A C7A C8A 0.6(6) . . . . ? C31A C6A C7A C8A -175.9(5) . . . . ? C6A C7A C8A C2A 0.0(6) . . . . ? C6A C7A C8A C41A 178.1(5) . . . . ? N1A C2A C8A C7A 174.6(5) . . . . ? N3A C2A C8A C7A -0.5(6) . . . . ? N1A C2A C8A C41A -3.6(9) . . . . ? N3A C2A C8A C41A -178.8(5) . . . . ? N2A C5A C11A C12A -159.8(5) . . . . ? C4A C5A C11A C12A 20.4(8) . . . . ? N2A C5A C11A C16A 24.4(8) . . . . ? C4A C5A C11A C16A -155.4(5) . . . . ? C16A C11A C12A C13A -1.9(7) . . . . ? C5A C11A C12A C13A -177.9(5) . . . . ? C11A C12A C13A C14A 1.9(8) . . . . ? C12A C13A C14A C15A -1.0(8) . . . . ? C13A C14A C15A C16A 0.1(8) . . . . ? C14A C15A C16A C11A -0.1(8) . . . . ? C12A C11A C16A C15A 1.0(7) . . . . ? C5A C11A C16A C15A 176.7(5) . . . . ? C4A C3A C21A C22A 160.3(5) . . . . ? C1A C3A C21A C22A -19.0(8) . . . . ? C4A C3A C21A C26A -17.0(8) . . . . ? C1A C3A C21A C26A 163.6(5) . . . . ? C26A C21A C22A C23A -2.1(8) . . . . ? C3A C21A C22A C23A -179.6(5) . . . . ? C21A C22A C23A C24A 1.9(8) . . . . ? C22A C23A C24A N24A 178.4(5) . . . . ? C22A C23A C24A C25A -1.5(8) . . . . ? N24A C24A C25A C26A -178.5(5) . . . . ? C23A C24A C25A C26A 1.4(8) . . . . ? C24A C25A C26A C21A -1.8(8) . . . . ? C22A C21A C26A C25A 2.0(7) . . . . ? C3A C21A C26A C25A 179.6(5) . . . . ? C25A C24A N24A C27A -8.1(8) . . . . ? C23A C24A N24A C27A 172.0(5) . . . . ? C25A C24A N24A C28A -170.2(5) . . . . ? C23A C24A N24A C28A 9.9(8) . . . . ? N3A C6A C31A C32A 24.3(8) . . . . ? C7A C6A C31A C32A -159.9(5) . . . . ? N3A C6A C31A C36A -155.6(5) . . . . ? C7A C6A C31A C36A 20.2(8) . . . . ? C36A C31A C32A C33A 0.7(7) . . . . ? C6A C31A C32A C33A -179.2(5) . . . . ? C31A C32A C33A C34A -0.9(8) . . . . ? C32A C33A C34A C35A 1.3(8) . . . . ? C33A C34A C35A C36A -1.6(8) . . . . ? C34A C35A C36A C31A 1.5(8) . . . . ? C32A C31A C36A C35A -1.0(7) . . . . ? C6A C31A C36A C35A 179.0(5) . . . . ? C7A C8A C41A C46A 168.1(5) . . . . ? C2A C8A C41A C46A -14.1(9) . . . . ? C7A C8A C41A C42A -12.5(8) . . . . ? C2A C8A C41A C42A 165.3(5) . . . . ? C46A C41A C42A C43A 0.4(7) . . . . ? C8A C41A C42A C43A -179.1(5) . . . . ? C41A C42A C43A C44A -1.5(8) . . . . ? C42A C43A C44A N44A -178.9(5) . . . . ? C42A C43A C44A C45A 2.0(7) . . . . ? N44A C44A C45A C46A 179.4(5) . . . . ? C43A C44A C45A C46A -1.5(7) . . . . ? C44A C45A C46A C41A 0.5(8) . . . . ? C42A C41A C46A C45A 0.1(7) . . . . ? C8A C41A C46A C45A 179.6(5) . . . . ? C43A C44A N44A C47A -178.6(4) . . . . ? C45A C44A N44A C47A 0.5(8) . . . . ? C43A C44A N44A C48A -2.5(7) . . . . ? C45A C44A N44A C48A 176.5(4) . . . . ? C2B N1B C1B N2B -3.5(7) . . . . ? C2B N1B C1B C3B -175.0(5) . . . . ? N1B C1B N2B C5B -171.6(4) . . . . ? C3B C1B N2B C5B 0.9(5) . . . . ? N1B C1B N2B B1B 4.9(7) . . . . ? C3B C1B N2B B1B 177.4(4) . . . . ? C5B N2B B1B F2B 54.6(7) . . . . ? C1B N2B B1B F2B -120.9(5) . . . . ? C5B N2B B1B F1B -67.8(7) . . . . ? C1B N2B B1B F1B 116.7(5) . . . . ? C5B N2B B1B N3B 173.3(4) . . . . ? C1B N2B B1B N3B -2.2(7) . . . . ? F2B B1B N3B C6B -70.2(7) . . . . ? F1B B1B N3B C6B 50.5(7) . . . . ? N2B B1B N3B C6B 171.8(4) . . . . ? F2B B1B N3B C2B 116.5(5) . . . . ? F1B B1B N3B C2B -122.8(5) . . . . ? N2B B1B N3B C2B -1.5(7) . . . . ? C1B N1B C2B N3B -0.6(8) . . . . ? C1B N1B C2B C8B -174.3(5) . . . . ? C6B N3B C2B N1B -171.7(5) . . . . ? B1B N3B C2B N1B 3.1(8) . . . . ? C6B N3B C2B C8B 2.9(5) . . . . ? B1B N3B C2B C8B 177.7(4) . . . . ? N1B C1B C3B C4B 171.4(5) . . . . ? N2B C1B C3B C4B -0.9(5) . . . . ? N1B C1B C3B C21B -5.0(8) . . . . ? N2B C1B C3B C21B -177.3(4) . . . . ? C1B C3B C4B C5B 0.6(5) . . . . ? C21B C3B C4B C5B 176.8(5) . . . . ? C1B N2B C5B C4B -0.5(5) . . . . ? B1B N2B C5B C4B -176.6(5) . . . . ? C1B N2B C5B C11B 176.8(5) . . . . ? B1B N2B C5B C11B 0.7(8) . . . . ? C3B C4B C5B N2B 0.0(6) . . . . ? C3B C4B C5B C11B -177.4(5) . . . . ? C2B N3B C6B C7B -2.3(6) . . . . ? B1B N3B C6B C7B -176.2(5) . . . . ? C2B N3B C6B C31B 176.1(4) . . . . ? B1B N3B C6B C31B 2.1(8) . . . . ? N3B C6B C7B C8B 0.7(6) . . . . ? C31B C6B C7B C8B -177.7(4) . . . . ? C6B C7B C8B C41B 176.9(5) . . . . ? C6B C7B C8B C2B 1.1(5) . . . . ? N1B C2B C8B C7B 172.1(5) . . . . ? N3B C2B C8B C7B -2.5(5) . . . . ? N1B C2B C8B C41B -3.8(8) . . . . ? N3B C2B C8B C41B -178.4(5) . . . . ? N2B C5B C11B C16B 22.3(8) . . . . ? C4B C5B C11B C16B -160.8(5) . . . . ? N2B C5B C11B C12B -156.8(5) . . . . ? C4B C5B C11B C12B 20.1(7) . . . . ? C16B C11B C12B C13B 0.6(7) . . . . ? C5B C11B C12B C13B 179.8(5) . . . . ? C11B C12B C13B C14B 0.0(8) . . . . ? C12B C13B C14B C15B 0.6(8) . . . . ? C13B C14B C15B C16B -1.7(8) . . . . ? C14B C15B C16B C11B 2.3(8) . . . . ? C12B C11B C16B C15B -1.7(8) . . . . ? C5B C11B C16B C15B 179.1(5) . . . . ? C4B C3B C21B C26B -21.0(8) . . . . ? C1B C3B C21B C26B 154.4(5) . . . . ? C4B C3B C21B C22B 164.2(5) . . . . ? C1B C3B C21B C22B -20.4(8) . . . . ? C26B C21B C22B C23B -1.3(7) . . . . ? C3B C21B C22B C23B 173.8(5) . . . . ? C21B C22B C23B C24B -1.4(8) . . . . ? C22B C23B C24B N24B -175.2(5) . . . . ? C22B C23B C24B C25B 3.7(7) . . . . ? N24B C24B C25B C26B 175.3(5) . . . . ? C23B C24B C25B C26B -3.5(8) . . . . ? C24B C25B C26B C21B 1.0(8) . . . . ? C22B C21B C26B C25B 1.5(7) . . . . ? C3B C21B C26B C25B -173.7(5) . . . . ? C23B C24B N24B C27B -174.4(5) . . . . ? C25B C24B N24B C27B 6.8(8) . . . . ? C23B C24B N24B C28B -3.6(8) . . . . ? C25B C24B N24B C28B 177.6(5) . . . . ? N3B C6B C31B C32B 28.4(8) . . . . ? C7B C6B C31B C32B -153.5(5) . . . . ? N3B C6B C31B C36B -153.5(5) . . . . ? C7B C6B C31B C36B 24.6(7) . . . . ? C36B C31B C32B C33B 0.1(7) . . . . ? C6B C31B C32B C33B 178.2(5) . . . . ? C31B C32B C33B C34B 0.1(8) . . . . ? C32B C33B C34B C35B -0.2(8) . . . . ? C33B C34B C35B C36B 0.1(8) . . . . ? C34B C35B C36B C31B 0.2(8) . . . . ? C32B C31B C36B C35B -0.3(7) . . . . ? C6B C31B C36B C35B -178.5(5) . . . . ? C7B C8B C41B C46B 170.9(5) . . . . ? C2B C8B C41B C46B -14.2(8) . . . . ? C7B C8B C41B C42B -9.8(8) . . . . ? C2B C8B C41B C42B 165.2(5) . . . . ? C46B C41B C42B C43B 3.4(7) . . . . ? C8B C41B C42B C43B -175.9(5) . . . . ? C41B C42B C43B C44B -0.9(8) . . . . ? C42B C43B C44B N44B 177.5(5) . . . . ? C42B C43B C44B C45B -1.7(7) . . . . ? N44B C44B C45B C46B -177.6(5) . . . . ? C43B C44B C45B C46B 1.7(7) . . . . ? C44B C45B C46B C41B 1.0(8) . . . . ? C42B C41B C46B C45B -3.5(7) . . . . ? C8B C41B C46B C45B 175.8(5) . . . . ? C43B C44B N44B C47B 179.3(4) . . . . ? C45B C44B N44B C47B -1.4(7) . . . . ? C43B C44B N44B C48B -0.2(7) . . . . ? C45B C44B N44B C48B 179.0(4) . . . . ?